HRID1382188

反应详情

EQUATION

反应方程式

HRID 1382188 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A process according to claim 1, wherein the compound of formula II is reacted with ethylene carbonate in the presence of a catalytic amount of tributylamine at a temperature between +130° C. and +150° C.; the resulting reaction mixture is treated with phosgene in the presence of a catalytic amount of dimethylformamide at a temperature between +70° C. and +90° C. yielding the compound of formula IV, which after purification is treated with 1 equivalent of chlorosulfonic acid or with a slight excess thereof in cyclohexane or n-decane at a temperature between +20° C. and +60° C.; neutralized with aqueous sodium hydroxide at a temperature between +50° C. and +90° C.; dechlorinated with hydrogen in the presence of an acid acceptor, in the pressure range from 1 to 5 bar at a temperature between +20° C. and +70° C. and in the presence of a 5% palladium on carbon catalyst; converted to the sulfonic acid chloride by treatment of the mixture with phosgene at a temperature between +60° C. and +120° C.; and subsequently reacted to the final product by treatment of the reaction mixture with an aqueous solution of ammonia.

WORKUP

后处理

  1. customafter purification
  2. customat a temperature between +20° C. and +60° C.