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    Purification of Progesterone Receptor Modulators
    5.
    发明申请
    Purification of Progesterone Receptor Modulators 审中-公开
    孕酮受体调节剂的纯化

    公开(公告)号：US20110178311A1

    公开(公告)日：2011-07-21

    申请号：US13078273

    申请日：2011-04-01

    申请人： Mahmut Levent ,  Panolil Raveendranath ,  Bogdan Wilk ,  Donald Carl Boop ,  Marinus Cornelis Hofman

    发明人： Mahmut Levent ,  Panolil Raveendranath ,  Bogdan Wilk ,  Donald Carl Boop ,  Marinus Cornelis Hofman

    IPC分类号： C07D403/10

    CPC分类号： C07D403/04

    摘要： Processes are provided for purifying a compound of the structure (I): wherein, A, B, T, Q and R1 are defined herein, and wherein the process includes dissolving the compound of formula I in a solution containing acetone, water and a base at about 30° C.; filtering the solution containing the compound of formula I at about 30° C.; and precipitating the purified compound of formula I by adjusting the filtered solution to an acidic pH. Desirably, the compound of formula I is 5-(2-thioxospiro[cyclohexane-1,3-[3H]indol]-5-yl)-1-methylpyrrole-2-carbonitrile or tanaproget.

    摘要翻译： 提供用于纯化结构（I）的化合物的方法：其中A，B，T，Q和R 1在本文中定义，并且其中所述方法包括将式I化合物溶解在含有丙酮，水和碱的溶液 在约30℃。 在约30℃下过滤含有式I化合物的溶液; 并通过将过滤的溶液调节至酸性pH而沉淀出纯化的式I化合物。 理想地，式I化合物是5-（2-噻吩并[环己烷-1,3- [3 H]吲哚] -5-基）-1-甲基吡咯-2-腈或十八碳炔。

    Process for preparing substituted 2,2'-methylene-bis-[6-(2H-benzotriazol-2-yl)-4-hydrocarbyl-phenols]
    7.
    发明授权
    Process for preparing substituted 2,2'-methylene-bis-[6-(2H-benzotriazol-2-yl)-4-hydrocarbyl-phenols] 失效
    取代的2,2'-亚甲基 - 双 - [6-（2H-苯并三唑-2-基）-4-烃基 - 酚]的制备方法]

    公开(公告)号：US5166355A

    公开(公告)日：1992-11-24

    申请号：US649972

    申请日：1991-02-04

    申请人： William E. Leistner ,  Semyon Moshchitsky ,  Mahmut Levent

    发明人： William E. Leistner ,  Semyon Moshchitsky ,  Mahmut Levent

    IPC分类号： C07C45/72 ,  C07C49/84 ,  C07D249/20

    CPC分类号： C07D249/20 ,  C07C45/72 ,  C07C49/84

    摘要： A method is described for preparing compounds of Formula I and Formula II: ##STR1## R.sub.1 is an alkyl group of one to twelve carbon atoms or a cycloalkyl group of five to eight carbons, X is chloro or hydrogen, and R.sub.2 is an alkoxy group having one to twelve carbons. In accordance with the method:(a) a bis(dialkylamino)methane is formed, preferably by reacting a dialkylamine of the formula HNR.sub.3 R.sub.4 (wherein R.sub.3 and R.sub.4 are independently alkyl groups having three or more carbons) and a solid formaldehyde material to produce the corresponding bis(dialkylamino)methane,(b) a monomer of Formula III or IV ##STR2## in which R.sub.1 is an alkyl group of one to twelve carbons or a cycloalkyl group of five to eight carbons, X is chloro or hydrogen and R.sub.2 is an alkoxy group having one to twelve carbon atoms, is mixed with an alkaline catalyst with heating at a temperature high enough to drive off the liquid formed in the reaction,(c) the product of steps (a) and (b) are combined and stirred at a temperature sufficient to drive the reaction for six to fourteen hours, and(d) thereafter the resulting compound of Formula I is collected.

    摘要翻译： 描述了制备式I和式II化合物的方法：R 1是1至12个碳原子的烷基或5至8个碳的环烷基，X是氯或氢，以及 R2是具有1〜12个碳原子的烷氧基。 根据以下方法：（a）形成双（二烷基氨基）甲烷，优选通过使式HNR 3 R 4的二烷基胺（其中R 3和R 4独立地为具有三个或更多个碳的烷基）和固体甲醛材料反应，生成 对应的双（二烷基氨基）甲烷，（b）式III或IV的单体IV，其中R 1是1至12个碳的烷基或5至8个碳的环烷基，X是氯 或氢，R2为具有1〜12个碳原子的烷氧基，与碱催化剂在足够高的温度下加热以除去反应中形成的液体，（c）步骤（a）和（ b）在足以驱动反应6至14小时的温度下混合并搅拌，然后收集所得到的式I化合物。

    Process for preparing 2,2'-methylene-bis(6-(2H-benzotriazol-2-yl)-4-hydrocarbyl phenols)
    10.
    发明授权
    Process for preparing 2,2'-methylene-bis(6-(2H-benzotriazol-2-yl)-4-hydrocarbyl phenols) 失效
    制备2,2'-亚甲基 - 双（6-（2H-苯并三唑-2-基）-4-烃基酚的方法）

    公开(公告)号：US5237071A

    公开(公告)日：1993-08-17

    申请号：US644299

    申请日：1991-01-22

    申请人： William E. Leistner ,  Semyon Moshchitsky ,  Mahmut Levent

    发明人： William E. Leistner ,  Semyon Moshchitsky ,  Mahmut Levent

    IPC分类号： C07D249/20

    CPC分类号： C07D249/20

    摘要： A method for preparing 2,2'-methylene-bis-[6-(2H)-benzotriazol-2-yl)-4-hydrocarbyl phenols] is disclosed. According to the process(i) formaldehyde, a dialkylamine and a 4-hydrocarbyl-6-benzotriazolyl phenol as monomer are mixed;(ii) the mixture is heated to a temperature high enough to remove the water produced by the reaction of the mixture;(iii) thereafter an alkaline catalyst is added with heating for several hours;(iv) the phenol compound precipitates when the reaction mixture is neutralized and solvent for the salt product of the neutralization reaction is added in an amount sufficient to permit stirring.The solid product produced is 2,2'-methylene-bis-[6-(2H-benzotriazol-2-yl)-4-hydrocarbyl phenol] having the formula I: ##STR1## in which each R group is an alkyl group of one to twelve carbons or a cycloalkyl group of five to eight carbons and X is chloro or hydrogen.

    摘要翻译： 公开了一种制备2,2'-亚甲基 - 双 - [6-（2H） - 苯并三唑-2-基）-4-烃基酚的方法]。 根据方法（i）甲醛，将二烷基胺和作为单体的4-烃基-6-苯并三唑基苯酚混合; （ii）将混合物加热到足够高的温度以除去由混合物反应产生的水; （iii）然后加热碱性催化剂数小时; （iv）当反应混合物中和时，酚化合物沉淀，并且以足以允许搅拌的量加入中和反应的盐产物的溶剂。 产生的固体产物是具有式I的2,2'-亚甲基 - 双[6-（2H-苯并三唑-2-基）-4-烃基苯酚]，其中每个R基团是 一至十二个碳或五至八个碳的环烷基，X是氯或氢。