专利号:EP-1546135-B1 优先权日:2002-07-16 标题:Novel synthesis of irbesartan 发明人:NISNEVICH GENNADY; RUKHMAN IGOR; PERTSIKOV BORIS; KAFTANOV JULIA; DOLITZKY BEN-ZION 权利人:TEVA PHARMA 摘要:Provided is a novel synthesis of irbesartan employing a phase transfer catalyst. Also provided is irbesartan having a fine particle size.
专利号:US-7312340-B2 优先权日:2003-02-05 标 题:Synthesis of 2-butyl-3-(1-trityl-1H-tetrazol-5-YL)biphenyl-4-YL)-1,3-diazaspiro[4,4]- non-ene-4-one 发明人:DOLITZKY BEN-ZION; KAFTANOV JULIA; PERTSIKOV BORIS; RUKHMAN IGOR; NISNEVICH GENNADY 权利人:TEVA PHARMA 摘要:Provided is a novel method of making 2-butyl-3-[[2′(1-trityl-1H-tetrazol-5-yl)biphen-4-yl]methyl]-1,3-diazaspiro[4.4]non-1-ene-4-one, which can be converted to irbesartan. Also provided are methods of making irbesartan.
专利号:US-5175302-A 优先权日:1987-07-13 标 题 :Nucleophilic fluoroalkylation of aldehydes 发明人:STAHLY G PATRICK 权利人:ETHYL CORP 摘要:Aryl difluoromethyl sulfone adds to aldehydes under phase transfer conditions to give novel substituted alcohols of the general formula n n RCH(OH)CF.sub.2 SO.sub.2 Ar (I) n n wherein R is an aryl, cycloaliphatic, sec- or tert-aliphatic, or heterocyclic group and Ar is an aryl group. The substituted alcohols of formula I are of particular utility as intermediates in the synthesis of a variety of useful end products. For example, the products of formula I may be utilized in desulfonylation reactions, oxidation reactions and fluorination reactions.
专利号:US-4999429-A 优先权日:1989-01-09 标 题 :Process for the preparation of α,α,β-1-trifluoro-1-olefinic derivatives 发明人:STAHLY G PATRICK 权利人:ETHYL CORP 摘要:Aryl difluoromethyl sulfone adds to aldehydes under phase transfer conditions to give novel substituted alcohols of the general formula n n RCH(OH)CF.sub.2 SO.sub.2 Ar (I) n n wherein R is an aryl, cycloaliphatic, sec- or tert-aliphatic, or heterocyclic group and Ar is an aryl group. The substituted alcohols of formula I are of particular utility as intermediates in the synthesis of a variety of useful end products. For example, the products of formula I may be utilized in desulfonylation reactions, oxidation reactions and fluorination reactions.
专利号:US-6326498-B1 优先权日:2001-03-13 标 题 :Process for the synthesis of 5-(2-flurophenyl)-1H-tetrazole 发明人:MALLADI PARDHASARADHI; KANTEVARI SRINIVAS; NAIR CHEMBUMKULAM KAMALAKSHYAM 权利人:COUNCIL SCIENT IND RES 摘要:The present invention discloses a process of the preparation of 5-(2-flurophenyl)-1H-tetrazole of the formula 2 by reacting 2-fluoro benzonitrile of the formula 1 n with an inorganic azide and an amine salt in an aromatic solvent, precipitating the product with hydrochloric acid and separating the precipitated product.
专利号:US-7741492-B2 优先权日:2005-02-28 标题:Method for obtaining a pharmaceutically active compound (Irbesartan) and its synthesis intermediate 发明人:HUGUET CLOTET JOAN; DALMASES BARJOAN PERE 权利人:INKE SA 摘要:It is provided a method for obtaining Irbesartan polymorph A, with few synthesis steps, by coupling the intermediate of formula (II) with the compound of formula (III), neutralising one of its alkaline salts in an aqueous medium and recrystallising the crude product obtained. The utilisation of said method obviates protection and deprotection of the tetrazole ring and is therefore of considerable interest for obtaining Irbesartan on a large industrial scale. The invention also refers to the synthesis intermediate of formula (II).
[参考文献]: V Balachandran, Et Al. Spectroscopic (Ft-Ir And Ft-Raman) Studies, Nbo, Homo-Lumo, Nmr Analyses And Thermodynamics Functions Of 5-Bromo-2-Methoxybenzaldehyde. Spectrochim Acta A Mol Biomol Spectrosc. 2013 Apr:106:262-74.
合成参考文献
参考文献:10.1107/s1600536811017910 摘要:Ban HY. (E)-N'-(5-Bromo-2-meth-oxy-benzyl-idene)isonicotinohydrazide. Acta Crystallogr Sect E Struct Rep Online. 2011 Jun 01;67(Pt 6):o1443.