HRID1978855

反应详情

EQUATION

反应方程式

HRID 1978855 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.36 g of 3-[3-(2-bromo-2-chlorocarbonylethenyl)-4-chlorophenyl]-2,4-dioxo-1-methyl-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine in 20 ml of tetrahydrofuran were added dropwise to a solution of 0.58 g of 2-ethylmercaptoethanol and 0.56 g of triethylamine in 30 ml of tetrahydrofuran, and stirring was carried out for 5 hours. 100 ml of water were added and the aqueous phase was extracted with twice 100 ml of dichloromethane. The combined organic phases were washed three times with water, dried with sodium sulfate and evaporated down. The solid residue was stirred with diisopropyl ether, removed, washed with diisopropyl ether and petroleum ether and dried.

WORKUP

后处理

  1. extractionthe aqueous phase was extracted with twice 100 ml of dichloromethane
  2. washThe combined organic phases were washed three times with water
  3. dry with materialdried with sodium sulfate
  4. customevaporated down
  5. stirringThe solid residue was stirred with diisopropyl ether
  6. customremoved
  7. washwashed with diisopropyl ether and petroleum ether
  8. customdried