HRID1639249

反应详情

EQUATION

反应方程式

HRID 1639249 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of [2-(2-fluorobenzoyl)-1H-pyrrol-1-yl]carbamic acid, ethyl ester (60.0 g, prepared from 1-amino-2-(2-fluorobenzyl)pyrrole and ethyl chloroformate in substantially the same manner as in Example 3) in 250 ml of ethanol was treated with a solution of potassium hydroxide (51 g) in 150 ml of water and then the mixture was heated at reflux for 1 hour. The ethanol was evaporated and the aqueous layer washed with 3×500 ml of ether. The aqueous phase was then adjusted to pH 5 with 6N HCl and the product collected by filtation. Oven drying yielded 20 g of a yellow powder, mp>300° C.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 1 hour
  3. customThe ethanol was evaporated
  4. washthe aqueous layer washed with 3×500 ml of ether
  5. customthe product collected by filtation
  6. customOven drying