HRID2351877

反应详情

EQUATION

反应方程式

HRID 2351877 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of 4.4 g of 2-[3-(3-cyanopropoxy)phenoxymethyl]quinoline 2.6 g of sodium azide and 2.1 g of ammonium chloride in 35 ml of dry dimethylformamide is heated at 140° C. for 18 hours. The reaction mixture is poured onto ice. A solution of 20 ml of 1N sodium hydroxide is added and the solution is extracted twice with ethyl acetate. Concentrated hydrochloric acid is added to acidify the aqueous portion. This is extracted twice with ethyl acetate, dried and evaporated to give 4.5 g of a tan solid. Recrystallization from ethyl acetate gives 1.5 g of pure product of M.P. 147°-149° C.

WORKUP

后处理

  1. additionThe reaction mixture is poured onto ice
  2. extractionthe solution is extracted twice with ethyl acetate
  3. additionConcentrated hydrochloric acid is added
  4. extractionThis is extracted twice with ethyl acetate
  5. customdried
  6. customevaporated