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    Method for producing alkenylthiophenols and their esters
    6.
    发明公开
    Method for producing alkenylthiophenols and their esters 失效
    Verfahren zur Herstellung von Alkenylthiophenolen und ihren Estern。

    公开(公告)号：EP0271307A2

    公开(公告)日：1988-06-15

    申请号：EP87310757.7

    申请日：1987-12-08

    申请人： HOECHST CELANESE CORPORATION

    发明人： Aslam, Mohammad ,  Graham, R. Russell ,  Davenport, Kenneth G.

    IPC分类号： C07C321/26 ,  C07C323/18 ,  C07C327/02 ,  C07C49/245

    CPC分类号： C07C323/00 ,  C07C45/46 ,  C07C45/54 ,  C07C327/00

    摘要： A method is provided for preparing alkenylthiophenols, e.g. para-vinylthiophenol, or their esters, e.g., para-vinylthiophenol acetate by reacting a hydroxy aromatic ketone, e.g., 4-hydroxyacetophenone (4-HAP) with an N,N-di(organo)thiocarbamoyl halide, e.g., N,N-dimethylthiocarbamoyl chloride (DMTC) to form an O-(acylaryl) N,N-di(organo)thiocarbamate, e.g., O-(4ʹ-acetophenyl) N,N-dimethylthiocarbamate, and pyrolytically rearranging the latter compound to form an S-(acylaryl) N,N-di(organo)thiocarbamate, e.g., S-(4ʹ-acetophenyl) N,N-dimethylthiocarbamate. In one procedure, the latter compound is directly reduced to form an S-(1-hydroxyalkylaryl) N,N-di(organo) thiocarbamate, e.g., S-[4ʹ-(1-hydroxyethyl)phenyl] N,N-dimethylthiocarbamate, which is either hydrolyzed to form a (1-hydroxyalkyl) thiophenol, e.g., 4ʹ-(1-hydroxyethyl) thiophenol, which, optionally after acylation of its thiol group, is dehydrated to form the alkenylthiophenol wherein the double bond is at the ring-bonded carbon atom, e.g., para-vinylthiophenol, or the S-(1-hydroxyalkylaryl) N,N-di(organo) thiocarbamate is dehydrated to form an S-(alkenylaryl) N,N-di(organo) thiocarbamate, e.g., S-(4-vinylphenyl) N,N-dimethylthiocarbamate which is hydrolyzed to form the alkenylthiophenol. In an alternative procedure, the S-(acylaryl) N,N-di(organo)thiocarbamate is hydrolyzed and the resulting thiol acylated with an acylating agent, e.g., acetyl chloride, to produce an acylthiophenol ester, e.g., 4-acetothiophenol acetate, which is then reduced and hydrolyzed to produce the (1-hydroxyalkyl) thiophenol. The latter compound is then dehydrated to produce the alkenylthiophenol, or acylated and dehydrated to produce the alkenylthiophenol thioester, as described in the first procedure.

    摘要翻译： 提供了制备烯基硫酚的方法，例如 通过使羟基芳族酮例如4-羟基苯乙酮（4-HAP）与N，N-二（有机）硫代氨基甲酰卤反应，例如N，N-二乙基苯硫酚或它们的酯，例如对乙烯基苯硫酚， 二甲基硫代氨基甲酰氯（DMTC）以形成O-（酰基芳基）N，N-二（有机））硫代氨基甲酸酯，例如O-（4'-乙酰苯基）N，N-二甲基硫代氨基甲酸酯，并热解重新排列后一种化合物以形成S- （酰基芳基）N，N-二（有机））硫代氨基甲酸酯，例如S-（4'-乙酰苯基）N，N-二甲基硫代氨基甲酸酯。 在一个步骤中，将后一种化合物直接还原形成S-（1-羟基烷基芳基）N，N-二（有机）硫代氨基甲酸酯，例如S- [4' - （1-羟乙基）苯基] N，N-二甲基硫代氨基甲酸酯 ，其被水解形成（1-羟基烷基）苯硫酚，例如4' - （1-羟乙基）苯硫酚，其任选地在其硫醇基团酰化后脱水以形成链烯基苯硫酚，其中双键位于 环状碳原子，例如对乙烯基苯硫酚或S-（1-羟基烷基芳基）N，N-二（有机））硫代氨基甲酸酯脱水形成S-（烯基芳基）N，N-二（有机））硫代氨基甲酸酯， 例如S-（4-乙烯基苯基）N，N-二甲基硫代氨基甲酸酯，其被水解形成烯基苯硫酚。 在另一种方法中，S-（酰基芳基）N，N-二（有机））硫代氨基甲酸酯水解，得到的硫醇用酰化剂（例如乙酰氯）酰化，得到酰基苯硫酚酯，例如4-乙酰苯硫酚乙酸酯， 然后将其还原并水解以产生（1-羟基烷基）苯硫酚。 然后将后一种化合物脱水以制备烯基苯硫酚，或者如第一步所述将其酰化和脱水以制备链烯硫基苯硫酚硫酯。

    METHOD FOR THE PREPARATION OF FLUTICASONE PROPIONATE
    7.
    发明公开
    METHOD FOR THE PREPARATION OF FLUTICASONE PROPIONATE 审中-公开
    VERFAHREN ZUR HERSTELLUNG VON FLUTICASONPROPIONAT

    公开(公告)号：EP1911741A1

    公开(公告)日：2008-04-16

    申请号：EP05781841.1

    申请日：2005-08-29

    申请人： Shanghai Aurisco International Trading Co., Ltd.

    发明人： CHU, Dingjun ,  ZHANG, Defa

    IPC分类号： C07C327/24 ,  C07C327/02 ,  C07J31/00

    CPC分类号： C07C327/24 ,  C07J31/00

    摘要： Taught is a method for preparing S-fluoromethyl-6α,9α- difluroro-11β-hydroxy-16α-methyl-17α- propionyloxy-3-oxoandrosta-1,4-diene-17β-carbothioate (fluticasone propionate). The present method is simple, convenient, and mild, yields highly pure product, and is suitable for use commercially on a large scale.

    摘要翻译： 教授是制备S-氟甲基-6±，9± - 二氟-D-12-羟基-16± - 甲基-17± - 丙酰氧基-3-氧代雄甾-1,4-二烯-17β-硫代磷酸酯（丙酸氟替卡松）的方法。 本发明方法简单，方便，温和，产生高纯度产品，适用于大规模商业应用。