HRID69558

反应详情

EQUATION

反应方程式

HRID 69558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Bromotrifluoroacetone (478 g, 1.05 eq) is added on a suspension of 5-(methoxymethyl)-1,3,4-thiadiazol-2-amine a25 (346 g, 1 eq) in 1,2-dimethoxyethane (6 l) at 20° C. The reaction mixture is heated to 80° C. until maximum conversion (<24 h). Water (4 l) is added to the reaction mixture at 32° C. and the expected compound crystallized out of the reaction mixture. The crystalline suspension is cooled to 10° C. to complete the crystallization process, filtered and the crystalline precipitate is washed with water (1.5 l) to afford 266 g of pure 2-(methoxymethyl)-6-(trifluoromethyl)imidazo[2,1-b][1,3,4]thiadiazole a28.

WORKUP

后处理

  1. customthe expected compound crystallized out of the reaction mixture
  2. temperatureThe crystalline suspension is cooled to 10° C.
  3. filtrationfiltered
  4. washthe crystalline precipitate is washed with water (1.5 l)