HRID1110123

反应详情

EQUATION

反应方程式

HRID 1110123 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

100 ml of n-tetrabutyl tin, then 120 mg of [benzyl (chloro) bis(triphenyl phosphine)]palladium were added to a solution of 40 ml of phenyl acetyl chloride in 500 ml of tetrahydrofuran. The mixture was stirred for 15 hours at reflux, filtered on clarcel and evaporated to dryness. The residue was distilled at 65° C. to 68° C. under 0.5 mm of mercury and the main fraction was chromatographed on silica (eluant: hexane - ethyl acetate (9-1)) to obtain 27.5 g of the desired product.

WORKUP

后处理

  1. temperatureat reflux
  2. filtrationfiltered on clarcel
  3. customevaporated to dryness
  4. distillationThe residue was distilled at 65° C. to 68° C. under 0.5 mm of mercury
  5. customthe main fraction was chromatographed on silica (eluant: hexane - ethyl acetate (9-1))