HRID1902654

反应详情

EQUATION

反应方程式

HRID 1902654 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A suspension of this amide (3.5 g) and triphenylphosphine (8.54 g) in carbon tetrachloride (10 ml), methylene chloride (20 ml) and triethylamine (2.3 ml) was stirred for 4 hours at room temperature. Ice (60 g) and 2 N hydrochloric acid (30 ml) were added, followed by sufficient chloroform to dissolve all the solid material. The solvent layer was washed with water, dried and evaporated, and the residue was crystallised from chloroform-petroleum spirit (60°-80° C.) and then from ethanol to give the title product (mp 177°-179° C.).

WORKUP

后处理

  1. dissolutionto dissolve all the solid material
  2. washThe solvent layer was washed with water
  3. customdried
  4. customevaporated
  5. customthe residue was crystallised from chloroform-petroleum spirit (60°-80° C.)