HRID2113892

反应详情

EQUATION

反应方程式

HRID 2113892 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 10.4 g (66.9 mmol) 1,3-dimethyl-pyrimidine-2,4,6-trione and 774 mg (0.67 mmol) tetrakis-(triphenylphosphine)-palladium in 100 ml dichloromethane was added dropwise a solution of 6.18 g (22.3 mmol) 1-[2-(4-allyloxy-2-fluoro-benzyloxy)-ethyl]-1H-[1,2,3]triazole in 30 ml dichloromethane and stirring was continued for 24 hours at 40° C. It was allowed to cool down over night. The reaction mixture was extracted with three 100 ml portions of sodium bicarbonate solution, the organic extract was dried, evaporated and purified by chromatography on silica (ethyl acetate/dichloromethane 3:7) to yield 2.97 g (56%) 3-fluoro-4-(2-[1,2,3]triazol-1-yl-ethoxymethyl)-phenol as oil.

WORKUP

后处理

  1. temperatureto cool down over night
  2. extractionThe reaction mixture was extracted with three 100 ml portions of sodium bicarbonate solution
  3. extractionthe organic extract
  4. customwas dried
  5. customevaporated
  6. custompurified by chromatography on silica (ethyl acetate/dichloromethane 3:7)