HRID1463841

反应详情

EQUATION

反应方程式

HRID 1463841 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3 g of benzo-1,2,3-thiadiazole-7-carboxylic acid chloride in 25 ml of dichloromethane are added dropwise at 15° C., with cooling and stirring, to a solution of 2.3 g of cinnamic alcohol, 3.5 g of triethylamine and a spatula tip of 4-dimethylaminopyridine in 13 ml of dichloromethane, the mixture is stirred for 16 hours at room temperature, ice-water is added, and the aqueous phase is extracted with dichloromethane. The extracts are washed with water, dried over Na2SO4 and concentrated by evaporation. The solid residue is triturated with a small amount of diethyl ether, yielding the title compound with a melting point of 70°-72° C.

WORKUP

后处理

  1. temperaturewith cooling
  2. extractionthe aqueous phase is extracted with dichloromethane
  3. washThe extracts are washed with water
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated by evaporation
  6. customThe solid residue is triturated with a small amount of diethyl ether