- A single isocyanate preparation method and system (by machine translation)
-
The invention relates to a single-isocyanate preparation method and system, the method using an excess of phosgene with the corresponding [...] phosgenation reaction, the obtained reaction solution through the mentioned after the hydrogen chloride escapes the carbonyl chloride, phosgene with the isocyanate to realize the complete separation of, excess phosgene can achieve the goal of recycling. In the phosgene escapes after cracking of the reaction liquid obtained by the pyrolysis gas inert solvent for [...], obtaining the corresponding isocyanate solution, follow-up separation can obtain the qualified isocyanate. The method for preparing the single isocyanate process with high yield and low solid the characteristics of the product waste. (by machine translation)
- -
-
Paragraph 0077; 0078; 0079; 0080; 0084
(2018/06/15)
-
- Continuous Flow Synthesis of Urea-Containing Compound Libraries Based on the Piperidin-4-one Scaffold
-
The advantages of performing reactions in continuous flow vs. the classic batch processes render flow chemistry a suitable technique for library synthesis. Inspired by our recent work to create fluorine-containing nitrogen heterocycles and by the potentia
- Riesco-Domínguez, Alejandra,Blanco-Ania, Daniel,Rutjes, Floris P. J. T.
-
p. 1312 - 1320
(2018/04/02)
-
- Synthetic method of isopropyl isocyanate
-
The invention discloses a synthetic method of isopropyl isocyanate, which includes steps of selecting isopropyl carbamyl chloride; reacting isopropyl carbamyl chloride in organic solvent for 4-15 hours at 50-160 DEG C under the catalysis of catalyst, thermally decomposing to obtain isopropyl isocyanate; the reaction equation is shown in the specification. The synthetic method has advanced technical route, and avoids virulent phosgene and superpalite; the synthetic method has advantages of being simple and safe in operation, high in reflection yield, low in production cost, basically free from three wastes, and great in practicing value and social and economic benefits.
- -
-
Paragraph 0028-0029
(2017/10/07)
-
- Synthesis of Amides and Phthalimides via a Palladium Catalyzed Aminocarbonylation of Aryl Halides with Formic Acid and Carbodiimides
-
A novel method for the preparation of amides and phthalimides has been developed. The process involves a palladium catalyzed aminocarbonylation of an aryl halide, using a carbodiimide and formic acid as the carbonyl source. Experimental data suggest that the mechanistic pathway for this process involves in-situ generation of carbon monoxide from the reaction of formic acid with a carbodiimide in the presence of a palladium catalyst. The method can be used to produce a variety of amides and N-substituted phthalimides efficiently.
- Seo, Yong-Sik,Kim, Dong-Su,Jun, Chul-Ho
-
supporting information
p. 3508 - 3512
(2016/12/26)
-
- Azabicyalo derivative as well as preparation and application thereof
-
The invention relates to an azabicyalo derivative as well as preparation and application thereof, and particularly discloses a compound with a structure shown in to the formula (A) or salt thereof acceptable in agricultural pharmacology. The compound in the formula (A) is described in the description in detail, and has an excellent killing effect on nematode.
- -
-
Paragraph 0178; 0179; 0180
(2016/10/07)
-
- (Tosylimino)phenyl-λ3-iodane as a reagent for the synthesis of methyl carbamates via hofmann rearrangement of aromatic and aliphatic carboxamides
-
A new, mild procedure for the Hofmann rearrangement of aromatic and aliphatic carboxamides using (tosylimino)phenyl-λ3-iodane, PhINTs, as a reagent is reported. Because of the mild reaction conditions, this method is particularly useful for the Hofmann rearrangement of substituted benzamides, which usually afford complex reaction mixtures with other hypervalent iodine oxidants. The mild reaction conditions and high selectivity in the reaction of carboxamides with PhINTs allow the isolation of the initially formed labile isocyanates or their subsequent conversion to stable carbamates by treatment with alcohols.
- Yoshimura, Akira,Luedtke, Matthew W.,Zhdankin, Viktor V.
-
experimental part
p. 2087 - 2091
(2012/05/05)
-
- Dicyclooctane Derivatives, Preparation Processes and Medical Uses Thereof
-
The present invention relates to new dicyclooctane derivates represented by general formula (I), preparation processes and pharmaceutical compositions containing them, and to uses for treatment especially for dipeptidyl peptidase inhibitor (DPPIV), in which each substituent group of general formula (I) is as defined in specification.
- -
-
Page/Page column 21
(2009/07/18)
-
- Synthesis and evaluation of structurally constrained imidazolidin derivatives as potent dipeptidyl peptidase IV inhibitors
-
To find potent and selective inhibitors of dipeptidyl peptidase IV (DPP-IV), we synthesized a series of 2-cyanopyrrolidine derivatives with constrained imidazolidin ring and tested their activities against DPP-IV. Most of them exhibited submicromolar inhibitory activities against DPP-IV. The most potent compound among these is (S)-1-(2-(2-(3-(3,4-dimethoxyphenyl)-2-oxoimidazolidin-1-yl)ethyl-amino)acetyl)pyrrolidine-2-carbonitrile (6n), which is a 2 nM DPP-IV inhibitor.
- Wang, Liutang,Zhang, Bin,Ji, Jianxin,Li, Bogang,Yan, Jufang,Zhang, Weiyu,Wu, Yong,Wang, Xuechao
-
experimental part
p. 3318 - 3322
(2009/12/01)
-
- DICYCLOOCTANE DERIVATES, PREPARATION PROCESSES AND MEDICAL USES THEREOF
-
The present invention relates to new dicyclooctane derivates represented by general formula (I), preparation processes and pharmaceutical compositions containing them, and to uses for treatment especially for dipeptidyl peptidase inhibitor (DPPIV), in which each substituent group of general formula (I) is as defined in specification
- -
-
Page/Page column 27-28
(2009/01/24)
-
- Organosilicon synthesis of isocyanates: II. Synthesis of aliphatic, carbocyclic, and fatty-aromatic isocyanates
-
Silylation of a series of aliphatic, carbocyclic, and fatty-aromatic amines gave the corresponding silyl derivatives whose yield depended on the electronic and steric structure of the substrate and the nature of the silylating agent. The yield of isocyanates obtained by phosgenation of the silyl derivatives under mild conditions decreased in going from aliphatic amines to benzylamines and rose as the length of the alkyl chain in fatty-aromatic amines extended. The most convenient procedure for the synthesis of low-boiling alkyl isocyanates was found to be based on the transformation of amines or ammonium salts into silyl or silyl silyl-carabamates, followed by pyrolysis of the latter in the presence of trichloro(phenyl)silane. Pleiades Publishing, Inc., 2006.
- Lebedev,Lebedeva,Sheludyakov,Ovcharuk,Kovaleva,Ustinova
-
p. 469 - 477
(2008/02/07)
-
- Azepinoindole derivatives as pharmaceutical agents
-
Compounds, compositions and methods for modulating the activity of receptors are provided. In particular, compounds and compositions are provided for modulating the activity of receptors and for the treatment, prevention, or amelioration of one or more symptoms of disease or disorder directly or indirectly related to the activity of the receptors.
- -
-
-
- Novel anticancer compounds : process for their preparation and pharmaceutical compositions containing them
-
The present invention relates to novel anticancer agents, their stereoisomers, their polymorphs, their pharmaceutically acceptable salts, and their pharmaceutically acceptable solvates. The present invention more particularly relates to novel derivatives of andrographolide, their stereoisomers, their polymorphs, their pharmaceutically acceptable salts, and their pharmaceutically acceptable solvates. The novel derivatives of andrographolide have the general formula (I).
- -
-
-
- Development of chiral N-alkylcarbamates as new leads for potent and selective H3-receptor antagonists: Synthesis, capillary electrophoresis, and in vitro and oral in vivo activity
-
Novel carbamates as derivatives of 3-(1H-imidazol-4-yl)propanol with an N-alkyl chain were prepared as histamine H3-receptor antagonists. Branching of the N-alkyl side chain with methyl groups led to chiral compounds which were synthesized stereospecifically by a Mitsunobu protocol adapted Gabriel synthesis. The optical purity of some of the chiral compounds was determined (ee > 95%) by capillary electrophoresis (CE). The investigated compounds showed pronounced to high antagonist activity (K(i) values of 4.1-316 nM) in a functional test for histamine H3 receptors on rat cerebral cortex synaptosomes. Similar H3-receptor antagonist activities were observed in a peripheral model on guinea pig ileum. No stereoselective discrimination for the H3 receptor for the chiral antagonists was found with the in vitro assays. All compounds were also screened for central H3-receptor antagonist activity in vivo in mice after po administration. Most compounds were potent agents of the H3-receptor-mediated enhancement of brain N(τ)- methylhistamine levels. The enantiomers of the N-2-heptylcarbamate showed a stereoselective differentiation in their pharmacological effect in vivo (ED50 of 0.39 mg/kg for the (S)-derivative vs 1.5 mg/kg for the (R)- derivative) most probably caused by differences in pharmacokinetic parameters. H1- and H2-receptor activities were determined for some of the novel carbamates, demonstrating that they have a highly selective action at the histamine H3 receptor.
- Sasse, Astrid,Kiec-Kononowicz, Katarzyna,Stark, Holger,Motyl, Malgorzata,Reidemeister, Sibylle,Ganellin, C. Robin,Ligneau, Xavier,Schwartz, Jean-Charles,Schunack, Walter
-
p. 593 - 600
(2007/10/03)
-
- Preparation of isocyanates from primary amines and carbon dioxide using Mitsunobu chemistry
-
Primary alkylamines 1 and hindered arylamines 1 give high yields of isocyanates 5 when reacted with carbon dioxide and the Mitsunobu zwitterions 4 generated from dialkyl azodicarboxylates and Bu3P in dichloromethane at - 78°C. Use of Ph3P still gave high yields of isocyanates from reactions of primary alkylamines, but only low yields were obtained from reactions of aromatic amines. Reactions which failed to give high yields of isocyanates gave either carbamoylhydrazines 6 and/or dicarbamoylhydrazines 10 and/or triazolinones 7. The triazolinones were shown to arise from reactions of reactive aryl isocyanates with the Mitsunobu zwitterion. The carbamoylhydrazines were shown not to arise from reaction of isocyanate with reduced dialkyl azodicarboxylates, and a mechanism for their formation is proposed. Single-crystal X-ray analyses confirmed the structures of 6, 7, and 10.
- Saylik, Dilek,Horvath, Michael J.,Elmes, Patricia S.,Jackson, W. Roy,Lovel, Craig G.,Moody, Keith
-
p. 3940 - 3946
(2007/10/03)
-
- A Mitsunobu-based procedure for the preparation of alkyl and hindered aryl isocyanates from primary amines and carbon dioxide under mild conditions
-
A Mitsunobu-based procedure for the preparation of alkyl and hindered aryl isocyanates in excellent yields from primary amines and carbon dioxide under very mild conditions is described.
- Horvath,Saylik,Elmes,Jackson,Lovel,Moody
-
p. 363 - 366
(2007/10/03)
-
- Reactivity of Carbamoyl Radicals. A New, General, Convenient Free-Radical Synthesis of Isocyanates from Monoamides of Oxalic Acid
-
A new, general, simple synthesis of isocyanates was developed by oxidation of monoamides of oxalix acid with peroxydisulfate catalyzed by Ag and Cu salts.The reaction was carried out in a two-phase system (water and an organic solvent), and it is suitable also for practical applications, due to the simple experimental conditions and the inexpensive as well as nontoxic reagents.The first example of homolytic intramolecular aromatic carbamoylation is also reported.
- Minisci, Francesco,Fontana, Francesca,Coppa, Fausta,Yan, Yong Ming
-
p. 5430 - 5433
(2007/10/02)
-
- Reaction of Oxalyl Chloride and Alkyloxalyl Chlorides with Isocyanates and Isothiocyanates
-
Alkyl and aryl isothiocyanates react with oxalyl chloride (1) on both double bonds of the heterocumulene to yield 3-alkyl- or 3-aryl-2,2-dichlorothiazolidine-4,5-diones 2.The two chlorines in these novel orthocarbonic acid derivatives are readily exchanged by alkoxy groups to yield 2,2-dialkoxythiazolidine-4,5-diones 3; hydrolysis of 2a (R=CH3) gave 3-methylthiazolidine-2,4,5-trione. 3-Substituted 5,5-dichlorooxazolidine-2,4-diones 8 and 5-chloro-5-alkoxyoxazolidine-2,4-diones 13 are obtained on reacting alkyl, aryl, and benzyl isocyanates with 1 and alkyloxalyl chloride, respectively.Structure assignment to these novel cycloadducts is based on IR, 1H NMR, and 13C NMR spectroscopic as well as X-ray crystallographic analysis.Formation of 8 and 13 is a stepwise process involving labile acyclic intermediates 7 and 12.The cyclizations to 8 and 13 take place only on the C=N bond of the isocyanate group.
- Richter, R.,Stuber, F. A.,Tucker, B.
-
p. 3675 - 3681
(2007/10/02)
-
- PHOTOCHEMICAL REACTIONS OF N-BENZOYLFORMYL-N-(PHENYLTHIOCARBONYL)-AMINES. A NOVEL PHOTOCYCLIZATION INVOLVING 1,4-PHENYLTHIO MIGRATION
-
Photolysis of N-benzoylformyl-N-(phenylthiocarbonyl)amines gave 5-(phenylthio)oxazolidine-2,4-diones which were produced by cyclization involving 1,4-phenylthio migration, accompanied by dimeric products (3) and diphenyl disulfide.
- Aoyama, H.,Sakamoto, M.,Omote, Y.
-
p. 1169 - 1170
(2007/10/02)
-
- FORMATION OF ISOCYANATES BY THERMAL REACTIONS OF 4-HYDROXY-5,5-DIMETHYL-4-PHENYLOXAZOLIDONE-2 DERIVATIVES
-
Thermolysis of 3N-substituted 4-hydroxy-5,5-dimethyl-4-phenyloxazolidone-2 derivatives, which were prepared by the reaction of carbon dioxide and α-bromoisobutyrophenone in the presence of primary amines, afforded corresponding isocyanates derived from 3N-substituents.
- Saito, Norio,Hatakeda, Kiyotaka,Ito, Shota,Asano, Takashi,Toda, Takashi
-
p. 905 - 906
(2007/10/02)
-
- Chemiluminescence of Imino-1,2-dioxetan Formed from Ketenimine and Singlet Oxygen
-
The chemiluminescent properties of several imino-1,2-dioxetans prepared by the photosensitized oxygenation of ketenimines at -78 degC, indicate that the energy level of the transition state for their decomposition to the corresponding ketones and isocyanates is low and that the decomposition proceeds via a biradical mechanism.
- Ito, Yoshikatsu,Yokoya, Hiroaki,Kyono, Kazuaki,Yamamura, Soichiro,Yamada, Yutaka,Matsuura, Teruo
-
p. 898 - 900
(2007/10/02)
-
- Process for the preparation of an aliphatic monoisocyanate
-
This invention relates to an improved process for the preparation of an aliphatic monoisocyanate from the corresponding carbamic acid chloride. The carbamic acid chloride is reacted with an active hydrogen compound. The reaction is conducted in the presence of a solvent which is inert under the reaction conditions. Addition compounds are formed with the elimination of hydrogen chloride. The addition compounds are subsequently decomposed by heat into the desired isocyanate with the mixture also containing the active hydrogen compound. The monoisocyanate is subsequently removed by distillation.
- -
-
-
- Manufacture of aliphatic or cycloaliphatic isocyanates
-
Aliphatic and cycloaliphatic isocyanates are manufactured by thermal decomposition of aliphatic or cycloaliphatic carbamic acid chlorides in the presence of an inert organic solvent of lower boiling point than that of the isocyanate formed. The decomposition is carried out in a reaction vessel surmounted by a rectifying unit, which in turn is surmounted by a reflux condenser, the isocyanate formed being condensed in the rectifying unit at a temperature above the boiling point of the solvent.
- -
-
-
- Manufacture of alkyl isocyanates
-
Aliphatic isocyanates are manufactured by thermal decomposition of aliphatic carbamic acid halides, an inert gas being passed in during the decomposition and being removed together with the hydrogen halide formed. The isocyanates which may be manufactured by the process of the invention, particularly ethyl isocyanate, n-propyl isocyanate and isopropyl isocyanate, are valuable starting materials for the manufacture of plant protection agents, pesticides, dyes, synthetic resins, plastics, hydrophobic agents for textiles, detergents, bleaches and adhesives.
- -
-
-
- Manufacture of aliphatic isocyanates
-
Aliphatic isocyanates are manufactured by thermal decomposition of aliphatic carbamic acid halides at a temperature not less than 25°C above their boiling points in the presence of higher-boiling organic solvents and subsequent isolation of the resulting aliphatic isocyanate from the decomposition mixture. The isocyanates which may be manufactured by the process of the invention are valuable starting materials for the manufacture of plant protection agents, pesticides, dyes, synthetic resins and plastics, hydrophobic agents for textiles, detergents, bleaches and adhesives.
- -
-
-
