HRID1904673

反应详情

EQUATION

反应方程式

HRID 1904673 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 was heated at 140° C. for 18 hours. The reaction mixture was poured onto ice. A solution of 20 ml of 1N sodium hydroxide was added and the solution was extracted twice with ethyl acetate. Concentrated hydrochloric acid was added to acidify the aqueous portion. This was extracted twice with ethyl acetate, dried and evaporated to give 4.5 g of a tan solid. Recrystallization from ethyl acetate gave 1.5 g of pure product of m.p. 147°-149° C.

WORKUP

后处理

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