HRID1614228

反应详情

EQUATION

反应方程式

HRID 1614228 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Tert-butyldimethylsilyl chloride (22.5 g) was added to a mixture of 3-hydroxypropiophenone (18.7 g), imidazole (21.3 g) and dimethylformamide (100 ml) and the solution was stirred at ambient temperature for 6 hours. The mixture was evaporated and the residue was partitioned between ethyl acetate and water. The organic layer was separated, washed with an aqueous sodium chloride solution, dried (Na2SO4) and evaporated. Petrol (b.p. 60°-80° C., 250 ml) was added to the residue, the resulting mixture was filtered and the filtrate was evaporated to give 3-(tert-butyldimethylsilyloxy)propiophenone as a pale yellow oil (31 g) which was used without further purification.

WORKUP

后处理

  1. customThe mixture was evaporated
  2. customthe residue was partitioned between ethyl acetate and water
  3. customThe organic layer was separated
  4. washwashed with an aqueous sodium chloride solution
  5. dry with materialdried (Na2SO4)
  6. customevaporated
  7. additionPetrol (b.p. 60°-80° C., 250 ml) was added to the residue
  8. filtrationthe resulting mixture was filtered
  9. customthe filtrate was evaporated