HRID1065088

反应详情

EQUATION

反应方程式

HRID 1065088 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of potassium cyanide (10.15 g, 0.156 mol) in water (31.25 ml) was added dropwise to a solution of 1-azabicyclo[2.2.2]-octan-3-one hydrochloride (25.0 g, 0.155 mol) in water (31.25 ml) at 0°-5°. Following the addition, the reaction mixture was stirred for 3 h and then filtered. The solid was washed with ice-cold water (2×15 ml) and was then dried over phosphorus pentoxide overnight, m.p. 155°-156°. Recrystallisation of a 1 g sample from dioxane gave pure 3-cyano-3-hydroxy-1-azabicyclo[2.2.2]octane, m.p. 172°-173°.

WORKUP

后处理

  1. additionthe addition
  2. filtrationfiltered
  3. washThe solid was washed with ice-cold water (2×15 ml)
  4. dry with materialwas then dried over phosphorus pentoxide overnight, m.p. 155°-156°
  5. customRecrystallisation of a 1 g sample from dioxane