HRID1667729

反应详情

EQUATION

反应方程式

HRID 1667729 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 5.09 g (10 mmole) of 2-(5-benzyloxy-2-nitro-phenylamino)-4-(3-chloro-phenyl)-thiazole-5-carboxylic acid ethyl ester (VI.25), 100 mL of tetrahydrofuran and 20 mL of 1M hydrochloric acid, was added portionwise, 10 g of zinc powder. The mixture was stirred at ambient temperature for 2 hours. The solid was removed by filtration, the filtrate was concentrated under reduced pressure and 200 mL of water was added to the residue. The pH was adjusted to 9 by addition of 15% sodium hydroxide. The precipitate was collected by filtration to give crude 2-(2-amino-5-benzyloxy-phenylamino)-4-(3-chloro-phenyl)-thiazole-5-carboxylic acid ethyl ester (VII.25). This material was carried through to next reaction without further purification.

WORKUP

后处理

  1. additionwas added portionwise
  2. customThe solid was removed by filtration
  3. concentrationthe filtrate was concentrated under reduced pressure and 200 mL of water
  4. additionwas added to the residue
  5. additionThe pH was adjusted to 9 by addition of 15% sodium hydroxide
  6. filtrationThe precipitate was collected by filtration