- Direct Carbonylation of Polychloroalkanes into Acid Chlorides Using Metallic Salts Ternary Systems: an Example of Multistep Catalysis
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A catalytic cycle for the direct carbonylation of CCl4 into CCl3COCl, catalysed by metallic salts mixtures. e.g.AlCl3/MCln/CuCl, under unexpectedly mild conditions, is proposed on the basis of FTIR, 17O and 27Al NMR spectroscopic studies.
- Monflier, Eric,Mortreux, Andre,Petit, Francis,Lecolier, Serge
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Read Online
- Synthesis and Fungitoxic Evaluation of Acylamino-1,2,4-Triazoles
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Ten different acylamino-1,2,4-triazoles were prepared by the reaction of differently substituted benzoyl chlorides and acetyl chlorides with 4-amino-1,2,4-triazole using catalytic amount of triethylamine. The synthesized compounds were characterized using UV, 1H-nuclear magnetic resonance spectroscopy, and infrared spectroscopy. All the compounds were tested for their fungicidal potential against three fungal species, that is, Fusarium verticillioides, Macrophomina phaseolina, and Rhizoctonia solani using poisoned food technique. The synthesized compounds were tested at various concentrations along with standard carbendazim 50 WP. The amides synthesized by reaction of substituted benzoyl chlorides and 4-amino-1,2,4-triazole exhibited greater fungicidal activity against all the tested fungi as compared to the amides synthesized using substituted acetyl chlorides. Among all the tested compounds, 4-nitro-N-(4-H-1,2,4-triazol-4-yl)benzamide showed the maximum fungicidal activity with the least median effective dose (ED50) values of 100, 93, and 146 μg ml-1 against F verticillioides, M. phaseolina, and R. solani, respectively. All the compounds were found to be less effective than the standard used.
- Kaur, Gurinderjit,Kaur, Harleen,Kaur, Pardeep,Sharma, Sunita,Singh, Ravneet
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p. 389 - 395
(2021/11/22)
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- A high-purity 3, 5, 6 - trichloro-pyridine -2 - sodium alcoholate production process (by machine translation)
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The present invention relates to the technical field of chemical material production, and in particular relates to a high-purity 3, 5, 6 - trichloro-pyridine - 2 - sodium alcoholate production process, comprises the following steps: chlorine acetyl chloride; preparing trichlor; addition cyclization: the protection of inert gas atmosphere by adding solvent, the pure product of the chloroacetyl chloride, acrylonitrile and catalyst, the temperature of the stirred to back flow, so that the reflux to return to below the liquid level, reduced pressure distillation, heat filter, the catalyst can be recycled for use, get filtrate for use; preparing 3, 5, 6 - trichloro-pyridine - 2 - sodium alcoholate crude; for preparing high-purity 3, 5, 6 - trichloro-pyridine - 2 - sodium alcoholate. The invention solves the problems in the prior art 3, 5, 6 - trichloro-pyridine - 2 - sodium alcoholate preparation technical difficulty is high, the yield is low and low purity of, the prepared 3, 5, 6 - trichloro-pyridine - 2 - sodium alcoholate has high purity, high yield and relatively shallow the advantages of luster, reasonable production process and is favorable for industrial production. (by machine translation)
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Paragraph 0046; 0064
(2019/04/04)
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- Synthesis method of chloroacetyl chloride
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The invention discloses a synthesis method of chloroacetyl chloride (ClCH2COCl). To be specific, the synthesis method is characterized in that an activated carbon loaded lewis acid catalyst is used for catalyzing gaseous acetyl chloride and chlorine to perform an alpha-halogenation reaction in a contact reactor to generate the chloroacetyl chloride. Lewis acid is specifically ferric chloride or aluminium chloride, and the consumption of the lewis acid is 1-7% of the total material input of acetyl chloride. The synthesis method disclosed by the invention is high in catalyst utilizing rate, highin selectivity, and less in byproducts, and the purity of a product is higher than or equal to 99.5%; the reaction is performed at low temperature; the energy consumption is low; the environmental pollution is small; and the reaction equipment structure is simple, and the operation is easy.
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Paragraph 0023; 0025
(2019/03/28)
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- A synthetic method of trichloroacetyl chloride
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A synthetic method of trichloroacetyl chloride is provided and belongs to the field of organic synthesis. The method includes steps of subjecting chlorine and chloroacetic acid in a melt state to a contact reaction to prepare a primary chlorination material, heating and reacting the primary chlorination material with sulfur monochloride and chlorine to prepare a secondary chlorination material, and heating and reacting the secondary chlorination material with chlorine under actions of a catalyst to obtain the trichloroacetyl chloride. The method synthesizes the trichloroacetyl chloride in a non-water system by utilizing the chloroacetic acid. The non-water system is adopted, thus avoiding generation of toxic and harmful compounds in a preparation process, avoiding a dewatering step, improving environment protection performance of the preparation process, simplifying the synthetic process and facilitating reduction of a synthesis cost.
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Paragraph 0033-0060
(2017/02/24)
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- A mild method for the replacement of a hydroxyl group by halogen. 1. Scope and chemoselectivity
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α-Chloro-, bromo- and iodoenamines, which are readily prepared from the corresponding isobutyramides have been found to be excellent reagents for the transformation of a wide variety of alcohols or carboxylic acids into the corresponding halides. Yields are high and conditions are very mild thus allowing for the presence of sensitive functional groups. The reagents can be easily tuned allowing therefore the selective monohalogenation of polyhydroxylated molecules. The scope and chemoselectivity of the reactions have been studied and reaction mechanisms have been proposed.
- Munyemana, Fran?ois,George, Isabelle,Devos, Alain,Colens, Alain,Badarau, Eduard,Frisque-Hesbain, Anne-Marie,Loudet, Aurore,Differding, Edmond,Damien, Jean-Marie,Rémion, Jeanine,Van Uytbergen, Jacqueline,Ghosez, Léon
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p. 420 - 430
(2015/12/31)
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- A method for the preparation of trichloroacetyl chloride with silicon tetrachloride (by machine translation)
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The invention discloses a method for the preparation of trichloroacetyl chloride with silicon tetrachloride, silicon tetrachloride used as acyl chloride reagent, and trichloro acetic acid in 60-70 °C reaction under 2-4 hours, generating acetic chloride, generated after the cure, the trichloro acetyl chloride and other products by distillation or extraction method for separating. The effective conversion of this invention and an organosilicon polycrystalline silicon production of by-product production in a large amount of silicon tetrachloride, trichlor-production with high added value; in the conversion treatment brought by the development of the production of polycrystalline silicon is difficult to control at the same time the by-product silicon tetrachloride, significantly reduces the cost of the preparation of trichloroacetyl chloride. (by machine translation)
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Paragraph 0028; 0029; 0030
(2016/11/17)
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- Synthesis, characterization and molecular structures of barium(II) trichloroacetate DME/1,4-dioxane compounds
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Two new barium(II) trichloroacetate compounds, [Ba(H2O)(DME) (μ-O2CCCl3)2]n (1) and [{Ba(H2O)2(diox)0.5(μ-O2CCCl 3)2}(diox)]n (2) were synthesized and characterized by elemental analyses, physiochemical studies, FT-IR, 1H NMR, thermogravimetric analyses (TG/DTG/DSC) and single crystal X-ray studies. The reaction of hydrated barium(II) trichloroacetate monohydrate with excess DME (1,2-dimethoxyethane) and diox (1,4-dioxane) in methanol at room temperature led to the isolation of the novel compounds 1 and 2, respectively. Bridging trichloroacetate groups are anticipated on the basis of FT-IR studies and this was confirmed by the X-ray studies. Both compounds dissociate to produce ions in water, as shown by molar conductance values. 1H NMR spectroscopy confirms that DME and 1,4-dioxane are coordinated to the metal ion in these compounds. Single crystal X-ray diffraction studies reveal that the barium cation is coordinated to nine O atoms in a deformed coordination polyhedron in both compounds. Structural data of barium(II) trichloroacetates compounds have been obtained for the first time in the present investigation.
- Singh, Sukhjinder,Saini, Deepika,Mehta,Kaur, Ravneet,Ferretti, Valeria
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scheme or table
p. 202 - 209
(2012/03/10)
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- Reaction of carboxylic acids with tetrachlorosilane
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Tetrachlorosilane reacted with carboxylic acids RCOOH (R = Me, Bu, t-Bu) to give the corresponding acid chlorides RCOCl in 75-95% yield. The reactions of SiCl4 with trichloroacetic and 2-fluorobenzoic acids (R = Cl 3C, 2-FC6H4) occurred more difficultly, presumably for steric reasons, and the yields of the corresponding acid chlorides were 11 and 22%, respectively. Tetrachlorosilane failed to react with stearic acid under analogous conditions. Products of the reactions of SiCl 4 with chloroacetic and benzoic acids RCOOH (R = ClCH2, Ph) were tetraacyloxysilanes Si(OCOR)4, and tetrakis(chloroacetoxy) silane was formed in almost quantitative yield. The reaction of SiCl4 with glutaric acid led to the formation of a rubber-like polymeric material with the composition C5H6Cl2O4Si. The effect of pKa values of carboxylic acids on the direction and mechanism of the examined reaction is discussed.
- Voronkov,Vlasov,Belousova,Grigor'Eva,Vlasova
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experimental part
p. 318 - 321
(2010/09/07)
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- Practical and chemoselective reduction of acyl chloride to alcohol by borohydride in aqueous dichloromethane
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A simple methodology for the reduction of acid chlorides to their corresponding alcohols has been developed. Various carboxylic acids were converted to alcohols in excellent yields using NaBH4-K2CO3 in a mixed solvent system of dichloromethane and water (1:1) in the presence of a phase-transfer catalyst at low temperature. The importance of the work is its simplicity, selectivity, excellent yield, and very short reaction time. This new reduction condition has proved to be an excellent chemoselective method for a range of acid chlorides in the presence of various functional groups.
- Rajan, Ramya,Badgujar, Sachin,Kaur, Kamaljit,Malpani, Yashwardhan,Kanjilal, Pranab R.
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experimental part
p. 2897 - 2907
(2010/11/18)
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- Reactions of chloroethenes with atomic chlorine in air at atmospheric pressure
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Relative rate method at the temperature of 298 K and pressure of 1013 hPa and GC-MS detection were used for the study of kinetics of the reactions of Cl atoms with H2C=CCl2, cis-ClHC=CHCl, trans-ClHC=CHCl, ClHC=CCl2, and Cl2C=CCl2. The reaction products were identified by FTIR spectroscopy. A mechanism for the atmospheric degradation of chloro-ethenes has been suggested.
- Morozov,Nielsen,Morozova,Vasiliev,Loukhovitskaya
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experimental part
p. 754 - 760
(2011/01/09)
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- The Interaction of Trihalogenoacetic Anhydrides and Trihalogenoacetyl Chlorides with Thymidine 5′-Phosphate as an Approach to New Activating Agents in the Phosphorylation Reactions for Nucleotides
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The interaction of thymidine 5′-phosphate with trichloroacetic anhydride, trichloroacetyl chloride, and tribromoacetyl bromide was studied in dimethylformamide and acetonitrile in the presence of tertiary amines. The first two reactions gave the mixed anhydride of trichloroacetic and thymidylic acids (acyl phosphate) as the major product and P1,P 2-dithymidine 5′-pyrophosphate as the byproduct. The third reaction proceeded by a more complicated mechanism and mainly led to substituted polyphosphates. The subsequent treatment of the reaction mixtures with morpholine resulted in thymidine 5′-phosphoromorpholidate in a high yield. The phosphorylating activities of the trichloroacetyl and tribromoacetyl phosphates were 77 and 89%, respectively.
- Bogachev,Ulanov
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- Spectroscopic and dielcometric study of the kinetics of alcoholysis of trichloroacetyl chloride with butanol
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The kinetics of alcoholysis of trichloroacetyl chloride with butanol in carbon tetrachloride were studied by dielcometry and IR spectroscopy. The reaction is reversible, and it involves intermediate formation of 1-butoxy-1,2,2,2-tetrachloroethanol and 1,1,2,2,2-pentachloroethanol.
- Varfolomeeva,Terent'ev,Bulanova
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p. 1799 - 1802
(2007/10/03)
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- Tetrachloroethylene oxide: hydrolytic products and reactions with phosphate and lysine.
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Tetrachloroethylene, or perchloroethylene (PCE), has considerable industrial use and is of toxicological interest because of a variety of effects. Most of the existing literature presents PCE oxide as a critical intermediate in the oxidative metabolism of PCE to Cl(3)CCO(2)H, oxalic acid, and products covalently bound to proteins, including trichloroacetyl derivatives of lysine. PCE oxide was synthesized by photochemical oxidation of PCE and characterized. Decomposition at neutral pH (t(1/2) = 7.9 min at 0 degrees C, 5.8 min at 23 degrees C, 2.6 min at 37 degrees C) yielded only trace ( approximately 1%) Cl(3)CCO(2)H; the major products identified were CO (73% yield) and CO(2) (63% yield). In phosphate buffer (0.10 M) a major product was identified as oxalyl phosphate. Oxalyl chloride also reacted to form CO and CO(2) in aqueous solution and to form oxalyl phosphate in neutral phosphate buffer. Oxalyl phosphate decomposed to oxalic acid (t(1/2) = 53 min at 37 degrees C) but did not react with lysine. Reaction of PCE oxide with free lysine yielded the oxalic acid amide derivatives of lysine plus lysine dimers in which cross-linking of the amino groups involved oxalo linkage. The reaction of PCE oxide with albumin yielded mainly N(6)-oxalolysine and some (5%) N(6)-trichloroacetyllysine. We propose a reaction pathway for PCE oxide based on our previous studies with trichloroethylene oxide, in which C-C bond scission is a major product of reaction in aqueous buffer and yields CO and CO(2). Oxalyl species are proposed as intermediates and prominent acylating species formed in the reactions of the epoxide. The formation of Cl(3)CCO(2)H in cytochrome P450 reactions is postulated to result from intramolecular migration within an enzyme intermediate.
- Yoshioka, Tadao,Krauser, Joel A,Guengerich, F Peter
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p. 1096 - 1105
(2007/10/03)
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- Heterogeneous photoreaction of tetrachloroethene-air mixture on halloysite particles
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The heterogeneous photodegradation of tetrachloroethylene in air proceeded on clay particles (halloysite) under photoillumination (> 300 nm) with an induction period. The reaction with the released chlorine atoms accelerated the photodegradation of tetrachloroethylene. The relative humidity and tetrachloroethylene partial pressure did not affect the induction period and the removal rate. Based on the diffuse reflectance UV-visible spectra and the physical properties of the halloysite particles, various tentative photoreaction mechanisms were proposed, e.g., the tetrachloroethylene-oxygen molecule charge-transfer complex. The photoreaction rate was estimated based on a simulated calculation, which can reproduce the tetrachloroethylene initial pressure dependence vs. time for tetrachloroethylene and its degradation products. Since the atmospheric lifetime of tetrachloroethylene via the gas-phase reaction with OH radicals is 140 days, potential photoreactions on the atmosphere-soils interface may affect the movement of tetrachloroethylene in the environment in the case that soils contain several weight percent of reactive clays, such as the halloysite particles.
- Kutsuna,Ibusuki,Takeuchi
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p. 2484 - 2489
(2007/10/03)
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- Acid fluorides and 1,1-difluoroethyl methyl ethers as new organic sources of fluoride for antimony pentachloride-catalyzed halogen-exchange reactions
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1,1-Difluoroethyl methyl ethers such as the commercial veterinary anesthetic methoxyflurane (2,2-dichoro-1,1-difluoroethyl methyl ether, 6) decompose in the presence of a catalytic amount of antimony pentachloride. The rate of decomposition is dependent upon the number and position of halogen atoms in the ether: a high degree of halogenation at the methyl group or at the 2-position of the ethyl group makes the ether less prone to decomposition. The decomposition products are acid fluorides and halogenated methanes. The fate of the antimony pentachloride is conversion to a fluorochloroantimony species which can be used in situ to selectively fluorinate a polychlorinated substrate. Thus, 1,2,2,2-tetrachloro-1-fluoroethyl methyl ether (1) is converted cleanly to the anesthetic compound 2,2,2-trichloro-1,1-difluoroethyl methyl ether (2) using 6 as the fluoride source, exploiting the difference in stability of 2 and 6 to the pentavalent antimony species. It is also demonstrated that the acid fluorides obtained from decomposition of the 1,1-difluoroethyl methyl ethers are fluoride sources for halex reactions.
- Ramig, Keith,Kudzma, Linas V.,Lessor, Ralph A.,Rozov, Leonid A.
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- Kinetics and mechanism of the thermal gas-phase oxidation of tetrachloroethene by molecular oxygen in presence of trifluoromethylhypofluorite, CF3OF
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The oxidation of tetrachloroethene by molecular oxygen in presence of CF3OF has been studied at 314.0, 324.2, 334.1 and 344.3 K. The initial pressure of CF3OF was varied between 2.0 and 8.2 Torr, that of CCl2CCl2 between 8.7 and 21.7 Torr, that of O2 between 33.2 and 730.7 Torr. Several runs were made adding N2 at pressure varying between 250.4 and 525.9 Torr. The major products were CCl3C(O)Cl and COCl2. CF3OCCl2C(O)Cl, CCl2FC(O)Cl, CF3OCCl2CCl2F and CCl2FCCl2F were formed in traces. The oxidation is a chain reaction. Its rate increases with total pressure. The following mechanism, where E = CCl2CCl2, R = CCl2FCCl2, CF3OCCl2CCl2 or CCl3CCl2, R′ = CCl2F, CF3OCCl2 or CCl3 and M = effective pressure, explains the experimental results: 1) CF3OF+E → R+CF3O 3, 7) R+O2+M → RO2+M 5) RO → R′C(O)Cl+Cl 9) CCl3CCl2O → CCl3C(O)Cl+Cl 11) CCl3+O2+M → CCl3O2+M 13) CCl3O → COCl2+Cl 15) R+CF3OF → RF+CF3O 2) CF3O+E → R 4, 8) 2RO2 → 2RO+O2 6) Cl+E → CCl3CCl2 10) CCl3CCl2O → CCl3+COCl2 12) CCl3O2+RO2 → CCl3O+RO+O2 14) 2R → recombination products, k9 = (3.0±1.4) × 1013 exp(-9.66±1 kcal mol-1/RT) s-1. by R. Oldenbourg Verlag, Muenchen 1998.
- Czarnowski, Joanna
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p. 183 - 197
(2007/10/03)
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- Dimethylformamide-Catalyzed Chlorination with Pentavalent Phosphorus Chlorides
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It is found that the chlorinating activity of pentavalent phosphorus chlorides is much increased by DMF. Treatment with phosphorus oxychloride in the presence of DMF was used to prepare 1,4-dichlorobutane from THF in 85% yield and carboxylic acid chlorides from the corresponding acids in ～92% yield.
- Kaabak,Baranov,Kalitina,Orlov
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p. 117 - 119
(2007/10/03)
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- Halogen atom transfer radical cyclization of N-allyl-N-benzyl-2,2-dihaloamides to 2-pyrrolidinones, promoted by Fe0-FeCl3 or CuCl-TMEDA
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The halogen atom transfer radical cyclization of a N-allyl-N-benzyl-2,2-dihaloamides to 2-pyrrolidinones has been carried out in high yields under mild conditions, in a reaction promoted by CuCl-TMEDA or Fe0-FeCl3 in acetonitrile or N,N-dimethylformamide, respectively.
- Benedetti, Miriam,Forti, Luca,Ghelfi, Franco,Pagnoni, Ugo Maria,Ronzoni, Roberto
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p. 14031 - 14042
(2007/10/03)
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- Process for the preparation of trichloroacetyl chloride
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The invention relates to a process for the preparation of trichloroacetyl chloride by reaction of acetyl chloride or acetaldehyde or chlorinated derivatives thereof with chlorine in the presence of active charcoal as the catalyst.
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- Atmospheric Chemistry of Pentachloroethane (CCl3CCl2H): Absorption Spectra of CCl3CCl2 and CCl3CCl2O2 Radicals, Kinetics of the CCl3CCl2O2 + NO Reaction, and Fate of the CCl3CCl2O Radical
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The absorption spectra of CCl3CCl2 and CCl3CCl2O2 radicals and the rate constant for the reaction of CCl3CCl2O2 radicals with NO were measured at 296 +/- 2 K using a pulse radiolysis technique.The absorption spectra were measured over the wavelength range 220-400 nm.At 230 nm ?(CCl3CCl2) = (271 +/- 84)E-20 cm2 molecule-1, and at 240 nm ?(CCl3CCl2O2) = (145 +/- 21)E-20 cm2 molecule-1.The reaction of F atoms with CCl3CCl2H was determined to have a rate constant of (2.3 +/- 1.6)E-12 cm3 molecule-1 s-1.The reaction of CCl3CCl2O2 with NO proceeds with a rate constant of (6.2 +/- 1.6)E-12 cm3 molecule-1 s-1.This reaction gives NO2 and CCl3CCl2O radicals.In the atmosphere, 85percent of the CCl3CCl2O radicals eliminate a Cl atom to give CCl3C(O)Cl, and the remaining 15percent decompose via C-C bond scission to give CCl3 radicals and COCl2.As part of the present work, relative rate techniques were used to measure rate constants at 296 +/- 2 K for the reactions of Cl and F atoms with CCl3CCl2H of (5.2 +/- 0.7)E-14 and (2.0 +/- 0.5)E-12 cm3 molecule-1 s-1, respectively.
- Moegelberg, Trine E.,Sehested, Jens,Nielsen, Ole J.,Wallington, Timothy J.
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p. 16932 - 16938
(2007/10/02)
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- Photooxidation of exhaust pollutants: III. Photooxidation of the chloroethenes: Degradation efficiencies, quantum yields and products
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The photochemical decomposition and oxidation of the chloroethenes C2H4-XClX (x=1-4) was investigated in the gas phase by irradiation with a low pressure mercury lamp in an oxygen atmosphere. Degradation efficiencies directly depend on the number of chlorine atoms both at 185 and 254 nm. The quantum yields for degradation increase from 2-3 for vinyl chloride to > 100 for tri- and tetrachloroethene at 185 nm in the 10-3 bar concentration range. At 254 nm we measured nearly time independent quantum yields of around 10 for tri- and 40 for tetrachloroethene. The photooxidation products and their mechanism of formation are discussed in detail.
- Guertler,Moeller,Sommer,Mueller,Kleinermanns
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p. 1671 - 1682
(2007/10/03)
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- Conversion of carboxylic acids to acyl chlorides with a hexaalkylguanidinium chloride catalyst
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Hexaalkylguanidinium chloride displays different behavior toward carboxylic acids depending on the acid strength.Its high catalytic activity for the condensation of carboxylic acids with phosgene or thionyl chloride using molecular and grafted catalyst forms is described.Keywords - hexaalkylguanidinium chloride / catalyst / carboxylic acids / chlorination / phosgenation / mechanism
- Gros, P.,Perchec, P. Le,Gauthier, P.,Senet, J. P.
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p. 554 - 561
(2007/10/02)
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- KINETICS OF THE NONCATALYTIC REACTION OF TRICHLOROACETYL CHLORIDE WITH 1-BUTANOL IN TOLUENE AND OF THE REACTION CATALYZED BY CARBOXYLIC ACIDS
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The kinetics of the reaction of trichloroacetyl chloride with 1-butanol were investigated in pure toluene and also in the presence of additions of acetic acid and its derivatives.The catalytic activity of the carboxylic acids decreases with increase in their acidity, and the rate constants are described by the Taft equation.The negative value of the reaction constant, consistent with catalysis of bifunctional nature, indicates that the basic center of the bifunctional catalyst has a predominating role in the case where the elimination of the leaving group in the transition state is hindered.
- Semenyuk, G. V.,Razumova, N. G.,Oleinik, N. M.
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- REAGENTS AND SYNTHETIC METHODS 21. THIONYL CHLORIDE/4-(N,N-DIMETHYLAMINO)PYRIDINE COMPLEX. A SIMPLE ONE-POT METHOD FOR ESTERIFICATION OF CARBOXYLIC ACIDS.
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Esters are obtained by a one-pot method, in which the carboxylic acid is first converted into its acyl chloride by means of thionyl chloride/4-(N,N-dimethylamino)pyridine complex as a new activating reagents.
- Arrieta, A.,Garcia, T.,Palomo, C.
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p. 1139 - 1146
(2007/10/02)
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- ISOMERIZATION OF CHLORINE-SUBSTITUTED α-OXIDES
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During the thermal and catalytic isomerization of chlorine-substituted epoxyethanes to the corresponding carbonyl compounds the reaction rate increases with increase in the number of chlorine atoms in the molecule.Active catalysts are amines, Lewis acids, and sulfuric acid but not hydrochloric acid and carboxylic acids) the type of catalyst (acid or base) affects the direction of isomerization in the unsymmetrical chloroepeoxyethanes.
- Voronina, T. A.,Chernyavskii, A. I.,Dobrov, I. V.,Poluektov, V. A.,Fomina, N. V.
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p. 801 - 805
(2007/10/02)
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- Derivatives of 1,3,5-Triazine : Part II - Reactions of Cyanuric Chloride, a New Condensing Agent
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Cyanuric chloride, a new condensing agent, has been found to be useful in the preparation of acid chlorides, amides and esters in good yields from carboxylic acids, picryl chloride from picric acid, and in bringing about the pinacol rearrangment of substituted ethanediol derivatives and lactonization of (R)-(+)-ricinelaidic acid.Treatment of cyanuric chloride with ethanol and formamide at room temperature gives triethyl orthoformate in 28percent yield.
- Lahoti, R. J.,Wagle, D. R.
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p. 852 - 855
(2007/10/02)
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- Process for preparing amides by reaction in presence of molecular sieve
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There is provided a process for preparing amides which comprises reacting an amine, or an amide, and an acid halide, or anhydride, in suitable molecular proportions, in an inert organic diluent, in the presence of an effective amount of a molecular sieve, until the reaction is completed, separating the molecular sieve, and recovering the amide from the organic mother liquor.
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- Novel dibenzo[a,g]quinolizinium compounds
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9-Hydroxydibenzo[a,g]quinolizinium compound of the formula: STR1 wherein R5, R6, R8 and R13 are each hydrogen or lower alkyl, and X- is a pharmaceutically acceptable anion. Additional substituent may be present on ring A and D. Betaines and 9-acylates are also provided. They inhibit growth of transplanted sarcoma or leukemia strains into mice.
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