HRID1594225

反应详情

EQUATION

反应方程式

HRID 1594225 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Water (50 ml) was added to a stirred suspension of 4-tert-butyl-2-(4-methyl-benzoylamino)-4H-pyrrolo[2,3-d]thiazole-6-carboxylic acid ethyl ester (4.0 g, 10.5 mmol) and lithium hydroxide (1.0 g, 42.6 mmol) in THF (105 ml). The mixture was held at reflux for 18 hours, cooled, diluted with water (200 ml), and washed with ethyl acetate. The aqueous phase was chilled, then acidified (6M HCl), with stirring, to precipitate product. The solid was filtered and dried to yield 3.14 g (84%) of the product. MS: M+H=358.

WORKUP

后处理

  1. temperatureat reflux for 18 hours
  2. temperaturecooled
  3. washwashed with ethyl acetate
  4. temperatureThe aqueous phase was chilled
  5. customto precipitate product
  6. filtrationThe solid was filtered
  7. customdried