HRID1589966

反应详情

EQUATION

反应方程式

HRID 1589966 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 1.96 g (10 mmoles) of allyl 2-fluoro-4-hydroxybenzoate, 1.53 ml (11 mmoles) of triethylamine and 25 ml of THF, there is slowly added a solution of 3 g (10 mmoles) of 3-(1-adamantyl)-4-methoxybenzoyl chloride in 50 ml of THF. The reaction medium is stirred at ambient temperature for 12 hours and then poured into water and extracted with ethyl ether. The organic phase is decanted, washed with water, dried on magnesium sulfate and evaporated. The resulting residue is purified by chromatography on a silica column, eluted by a 50:50 mixture of dichloromethane and hexane. After evaporation of the solvents, 3.63 g (78% yield) of the expected ester having a melting point of 102°-104° C.

WORKUP

后处理

  1. extractionextracted with ethyl ether
  2. customThe organic phase is decanted
  3. washwashed with water
  4. customdried on magnesium sulfate
  5. customevaporated
  6. customThe resulting residue is purified by chromatography on a silica column
  7. washeluted by a 50:50 mixture of dichloromethane and hexane