HRID1609298

反应详情

EQUATION

反应方程式

HRID 1609298 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In 15 ml of N,N-dimethylformamide was dissolved 1.2 g of 4-[2-[2-(1H-tetrazol-5-yl)phenylthio]phenylcarbamoyl]p-henoxyacetic acid (prepared in Example 6), followed by addition of 0.44 g of N,N'-carbonyldiimidazole with ice-cooling and stirring. The mixture was stirred with ice-cooling for 20 minutes, then 0.42 g of N,N-dimethylglycolamide was added, and the mixture was stirred at room temperature overnight. This reaction mixture was acidified with acetic acid and diluted with water and the crystals separated out therefrom were collected by filtration and recrystallized from N,N-dimethylformamide-ethyl acetate to give 0.55 g of the title compound as white crystals.

WORKUP

后处理

  1. temperaturecooling
  2. stirringThe mixture was stirred with ice-
  3. temperaturecooling for 20 minutes
  4. stirringthe mixture was stirred at room temperature overnight
  5. customthe crystals separated out
  6. filtrationtherefrom were collected by filtration
  7. customrecrystallized from N,N-dimethylformamide-ethyl acetate