HRID1721949

反应详情

EQUATION

反应方程式

HRID 1721949 的结构方程式

PROCEDURE

实验过程

A mixture of 100 mg of 4-hydroxy-acetophenone, 96 mg of n-tetrabutylammonium acid sulfate, 1.5 ml of 50% sodium hydroxide solution, 3 ml of benzene, 1.5 ml of acetonitrile and 0.2 ml of 2-chloroethyl p-toluene sulfonate was refluxed for 18 hours under an inert atmosphere and the decanted phase was extracted with benzene. The organic phase was washed with water, dried over a deshydrant and evaporated to dryness under reduced pressure. The residue was chromatographed over silica and eluted with dichloroethane to obtain 127 mg of 1-[4-(2-chloroethoxy)-phenyl]-ethanone melting at ≃62° C.

WORKUP

后处理

  1. temperaturewas refluxed for 18 hours under an inert atmosphere
  2. extractionthe decanted phase was extracted with benzene
  3. washThe organic phase was washed with water
  4. customdried over a deshydrant
  5. customevaporated to dryness under reduced pressure
  6. customThe residue was chromatographed over silica
  7. washeluted with dichloroethane