HRID893321

反应详情

EQUATION

反应方程式

HRID 893321 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Heat a mixture of the amide from step A (10.0 g), phosphorous pentoxide (25 g), phosphorous oxychloride (15 mL) and xylene (250 mL) at reflux for 2 h. Cool the reaction mixture, slowly add water (500 mL), basify using NaOH and extract with benzene. Concentrate the benzene extract to a residue and triturate with diethyl ether to give 6-methyl-7-methoxy-1-[2-(4-chlorophenyl)ethyl]-3,4-dihydroisoquinoline (4.95 g), mp=122°-124° C.

WORKUP

后处理

  1. temperatureHeat
  2. temperatureat reflux for 2 h
  3. extractionextract with benzene
  4. concentrationConcentrate the benzene
  5. extractionextract to a residue
  6. customtriturate with diethyl ether