HRID892251

反应详情

EQUATION

反应方程式

HRID 892251 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 28.46 g (0.182 mol) 1,3-dimethyl-pyrimidine-2,4,6-trione and 1.81 g (1.57 mmol) tetrakis-(triphenylphosphine)-palladium in 600 ml dichloromethane was added dropwise a solution of 17.70 g (60.75 mmol) 1-[2-(4-allyloxy-phenylmethanesulfinyl)-ethyl]-1H-[1,2,3]triazole and stirring was continued for 6 hours at 45° C. It was allowed to cool down over night. The reaction mixture was extracted with three portions of sodium bicarbonate solution, then the aqueous phase was adjusted to pH 1 and extracted three times with ethyl acetate. The organic extract was dried and evaporated to yield 12.6 g (83%) 4-(2[1,2,3] triazol-1-yl-ethanesulfinylmethyl)-phenol as white solid.

WORKUP

后处理

  1. temperatureto cool down over night
  2. extractionThe reaction mixture was extracted with three portions of sodium bicarbonate solution
  3. extractionextracted three times with ethyl acetate
  4. extractionThe organic extract
  5. customwas dried
  6. customevaporated