HRID462255

反应详情

EQUATION

反应方程式

HRID 462255 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3,5-Dibenzylidene-4-piperidone, hydrochloride (10.0g) is reacted with 5.8 g of 70% aqueous 2,2,2-trifluoroethylhydrazine in 220 ml of methanol at reflux for 4 hours. Evaporation of the methanol on a rotary evaporator leaves 14 g of a foamy residue which crystallizes when triturated with 50 ml of boiling acetonitrile to yield (after cooling for about 16 hours) 10.3 g of material, melting point 206°-209° C (sintering at 195° C). Crystallization from 80 ml of ethanol yields 6.7 g of product, melting point 207°-209° C, sintering at 196° C.

WORKUP

后处理

  1. temperatureat reflux for 4 hours
  2. customEvaporation of the methanol
  3. customon a rotary evaporator