- Synthesis of chlorinated alkylbibenzyls and 9-chlororetene
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The synthesis of chlorinated alkylbibenzyls and 9-chlororetene is described. These compounds were synthesized for use as model compounds in analytical and toxicological characterization. The structures of the synthesized model compounds found to be very similar to those indentified in pulp mill effluent and products. The (1)H NMR and mass spectral data for the compounds are also reported.
- Nevalainen, T.
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- Preparation method of P-isopropyl benzaldehyde and from isopropylbenzene
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The invention provides a method for preparing p-isopropylbenzaldehyde and from isopropylbenzaldehyde, and the preparation method comprises the following steps of: one step. The method comprises the following steps: adding cumene, an aldehyde solution, dropwise adding hydrochloric acid, heating to 80 - 88 °C after charging, and separating the phase to obtain the organic phase. The method comprises the following steps: uniformly mixing the inorganic base, the water and the phase transfer catalyst into a hydrolysis solution, adding the organic phase obtained in the step, and carrying out phase separation and purification under stirring to obtain p-isopropylbenzyl alcohol. Step III. The method comprises the following steps: adding hydrogen peroxide to isopropyl benzyl alcohol, a catalyst and a phase transfer catalyst obtained in the steps of oxidation and adding hydrogen peroxide, filtering and separating the filtrate to obtain crude aldehyde crude product and purifying to obtain p-propyl benzaldehyde. The preparation method has the advantages of being low in cost, good in process selectivity, mild in process condition and easy to realize industrialization.
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Paragraph 0058-0061; 0066-0068; 0072-0074; 0079-0081; ...
(2021/10/30)
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- Triazole derivative as well as preparation method and application thereof
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The invention relates to a triazole derivative as well as a preparation method and application thereof, which belong to the technical field of organic synthetic drugs. The structure of the triazole derivative is shown as a formula I. In the formula I, R1 and R2 are H, Cl, Br,-CF3,-CH(CH3)2 or -OCH3, and R1 and R2 are not H at the same time. R3 is -CH2 or -COCH2; X and Y are N or C, X and Y are not C at the same time, and X and Y are not N at the same time. The triazole derivative disclosed by the invention has a certain inhibition effect on germs of various crop diseases. Small toxic andside effects on plants are achieved. The preparation method of the triazole derivative is simple.
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Paragraph 0053-0055; 0065-0066; 0068
(2020/06/09)
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- An efficient and convenient chloromethylation of some aromatic compounds catalyzed by zinc iodide
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Treatment of a series of aromatic hydrocarbons and O-carbethoxy phenol substrates with a mixture of chlorosulfonic acid and dimethoxymethane in CH2Cl2 catalyzed by zinc iodide affords the corresponding chloromethyl derivatives in good to excellent yields.
- Tang, Jian,Liu, Hongtao,Zhou, Jing,Zhang, Xingxian
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- A practical and convenient Blanc-type chloromethylation catalyzed by zinc chloride under solvent-free conditions
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Chloromethylation of various aromatic hydrocarbons and substituted phenolic derivatives with dimethoxymethane and chlorosulfonic acid was carried out in the presence of 10 mol% of ZnCl2 in a mild and efficient manner under solvent-free conditions. In addition, 2,6-dimethyltyrosine was synthesized in high yield via this protocol.
- Tang, Jian,Liu, Hongtao,He, Kailun,Zhang, Xingxian
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p. 925 - 932
(2019/03/17)
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- NMP-mediated chlorination of aliphatic alcohols with aryl sulfonyl chloride for the synthesis of alkyl chlorides
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NMP-mediated chlorination of aliphatic alcohols has been developed for the synthesis of alkyl chlorides. This facile, efficient and practical approach used simple and readily available aryl sulfonyl chlorides as the chlorination reagent for the construction of C–Cl bond in good to excellent yields with mild conditions and broad substrate scope.
- Zheng, Dagui,Mao, Liu-Liang,Zhu, Xian-Hong,Zhou, An-Xi
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supporting information
p. 2793 - 2800
(2018/11/06)
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- Syntheses of 7-Substituted Anthra[2,3- b]thiophene Derivatives and Naphtho[2,3- b:6,7- b']dithiophene
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7-R-Anthra[2,3-b]thiophene derivatives (1, R = H, Me, i-Pr, or MeO) are prepared in three steps (in average overall yield >50%) starting from (E)-4-RC6H4CH2(HOCH2)C=CI(CH2OH). The latter are commercial or readily prepared from 2-butyne-1,4-diol and ArCH2Cl (both costing 1 cent/mmol) at 10 g scales. These allow for the selective formation of (otherwise unattainable) higher solubility 7-derivatives. Similar methods allow for the preparation of naphtho[2,3-b:6,7-b']dithiophene 2 using equally low-cost starting materials.
- Al-Jumaili, Mustafa A.,Woodward, Simon
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p. 11437 - 11445
(2018/09/06)
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- CATALYST
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A catalyst in solid particulate form free from an external carrier material comprising (i) a complex of formula (I) wherein M is zirconium or hafnium; each X is a sigma ligand; L is a divalent bridge selected from -R'2C-, -R'2C-CR'2-, -R'2Si-, -R'2Si-Si R'2-, -R'2 Ge-, wherein each R' is independently a hydrogen atom, C1-20-alkyl, tri(C1-20-alkyl)silyl, C6-20-aryl, C7-20-arylalkyl or C7-20-alkylaryl; R2 is a C1-20-hydrocarbyl radical; R2' is a C1-20-hydrocarbyl radical;R6 is a linear or branched aliphatic C1-20-hydrocarbyl group, SR9or OSR9;R6' is a linear or branched aliphatic C1-20-hydrocarbyl group, SR9'or OR9'; with the proviso that neither R6 or R6' represents a group having a quaternary carbon atom directly attached to the indenyl ring; R9 is a C1-20-hydrocarbyl group;R9' is a C1-20-hydrocarbyl group; Ar is a C6-12-aryl or C5-12-heteroaryl group optionally carrying one or more substituents R8; Ar' is a C6-12-aryl or C5-12-heteroaryl group optionally carrying one or more substituents R8';each R8 is a C1-20-hydrocarbyl group;each R8' is a C1-20 -hydrocarbyl group;wherein at least two of R2 and R2'; R6 and R6'; or Ar and Ar' are the same;and (ii) a cocatalyst comprising a compound of a group 13 metal, e.g. Al or boron.
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Page/Page column 54
(2014/07/08)
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- Copper-catalyzed cyanation of benzyl chlorides with non-toxic K 4[Fe(CN)6]
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Copper-based catalysts were firstly introduced into the cyanation of benzyl chlorides with non-toxic K4[Fe(CN)6]. The presented method avoids the use of extremely poisonous alkali cyanides and precious palladium catalysts. No other reagent apart from CuI, K4[Fe(CN) 6] and toluene was used in the cyanation, showing that the presented protocol is simple and practical. A series of benzyl chlorides were smoothly cyanated in up to 85% yield under the optimal conditions.
- Ren, Yunlai,Dong, Chuanhua,Zhao, Shuang,Sun, Yanpei,Wang, Jianji,Ma, Junying,Hou, Chaodong
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supporting information; body text
p. 2825 - 2827
(2012/07/17)
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- Pd-catalyzed cyanation of benzyl chlorides with nontoxic K 4[Fe(CN)6]
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Non-toxic K4[Fe(CN)6] was demonstrated to be effective as a green cyanating agent for the cyanation of alkyl halides using PPh3/Pd(OAc)2 as a catalyst system. The presented method allowed a series of benzyl chlorides to be smoothly cyanated in up to 88% yield. In order to avoid or suppress the deactivation of the catalyst, the reaction was required to be performed in a stringent inert ambiance.
- Ren, Yunlai,Yan, Mengjie,Zhao, Shuang,Sun, Yanpei,Wang, Jianji,Yin, Weiping,Liu, Zhifei
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supporting information; body text
p. 5107 - 5109
(2011/10/05)
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- An inexpensive and convenient procedure for chloromethylation of aromatic hydrocarbons by phase transfer catalysis in aqueous media
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Reaction of aromatic hydrocarbons catalyzed by a novel catalytic system consisting of zinc chloride, acetic acid, sulfuric acid and PEG-800 in aqueous media under PTC conditions results in chloromethylation in good to excellent yield.
- Hu, Yu Lin,Lu, Ming,Ge, Qiang,Wang, Peng Cheng,Zhang, Sheng Bin,Lu, Ting Ting
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experimental part
p. 97 - 102
(2010/08/05)
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- BENZODIAZEPINONE COMPOUNDS USEFUL IN THE TREATMENT OF SKIN CONDITIONS
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The present invention provides a family of benzodiazepinone compounds and pharmaceutical compositions thereof. The present invention also provides methods of treating certain skin conditions, e.g., atopic dermatitis, rosacea, or psoriasis, by administering a benzodiazepinone and methods of reducing the proliferation of keratinocyte cells by exposing such cells to a benzodiazepinone.
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Page/Page column 17
(2009/05/28)
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- Interpretation of retention indices in gas chromatography for establishing structures of isomeric products of alkylarenes radical chlorination
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By an example of previously uncharacterized products obtained by alkylarenes radical chlorination was demonstrated that combination of various interpretation methods applied to the retention indices (RI) in the gas chromatography on the standard nonpolar phases (comparison of RI of products and initial compounds, characteristics of succession of the chromatographic elution of the structural isomers with the use of estimation of molecular dynamic parameters, application of the additive schemes to RI calculation, and using of structural analogy CH3?Cl for testing the results obtained) permitted unambiguous identification of the structure even without data of mass spectrometry.
- Zenkevich
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p. 270 - 280
(2007/10/03)
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- Conformational analysis of some 5-substituted 5H-dibenzo[a,d]-cycloheptenes
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Conformations and inversion barriers of 5H-dibenzo[a,d]cycloheptene (1a), 5-amino-5H-dibenzo[a,d]cycloheptene (1b), 5-chloro-5H-dibenzo[a,d]cycloheptene (1e), 5-hydroxy-5H-dibenzo[a,d]cycloheptene (1d), 5-methyl-5H-dibenzo[a,d]cycloheptene (1f), N-benzyl-5H-dibenzo[a,d]cyclohepten-5-imine (2) and N-(5H-dibenzo[a,d]cyclohepten-5-yl)benzylideneamine (1c) have been studied by means of dynamic nuclear magnetic resonance spectroscopy (DNMR) techniques, and comparison of the experimentally derived thermodynamic parameters was made with MM3, PM3 and ab initio calculated results. Attempts to determine the inversion barrier of 3-isopropyl-5H-dibenzo[a,d]cyclohepten-5-one (3) failed.
- Hjelmencrantz, Anders,Friberg, Annika,Berg, Ulf
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p. 1293 - 1300
(2007/10/03)
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- Improved selectivity in the chloromethylation of alkylbenzenes in the presence of quaternary ammonium salts
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Improved yield and selectivity in the chloromethylation of aromatic hydrocarbons in the presence of several phase transfer catalysts are reported. The best yield (98%) and selectivity (p/o ratio = 8.2) were obtained in the chloromethylation of cumene in the presence of a classical micellar catalyst.
- Selva,Trotta,Tundo
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p. 1003 - 1004
(2007/10/02)
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- Perfume compositions as well as perfumed articles and materials containing alkyl substituted benzyl cyanides as a fragrance
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Use of one or more alkyl substituted benzyl cyanides having the formula STR1 in which R1 and R2 each may represent a hydrogen atom or a methyl group and R3 represents a branched alkyl group having at most 6 carbon atoms as a perfume component in perfume compositions and in imparting perfume notes to articles for example soaps, cleaning preparations and cosmetic compositions.
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- Unidirectional Dieckmann Cyclizations on a Solid Phase and in Solution
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Dieckmann cyclization of 2percent divinylbenzene-copolystyrene resin alkyl pimelates and analogous benzyl alkyl pimelates is reported.The use of uniquely single-labeled dioate esters has allowed analysis of the direction of closure via decarboxylation of the keto ester products.The influence of steric factors on the competition between enolate condensation and transesterification and upon the direction of closure of the cyclization has been evaluated, and the conditions for achieving >99percent regioselective closure are described.Modifications in the conditions of solid-phase peptide synthesis required for successful high-temperature enolate cyclization have been developed and the results are compared to solution reactions of benzyl alkyl esters under similar conditions.The resin attachment afforded a clear benefit over the benzyl models and greatly simplified isolation and purification of the resulting β-keto esters.
- Crowley, John I.,Rapoport, Henry
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p. 3215 - 3227
(2007/10/02)
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- Insect maturation inhibitors
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Certain arylterpenoid compounds having excellent potential as insect control agents. The compounds are highly active as eclosion inhibiting agents against four species of flies and three species of mosquito.
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