HRID2163438

反应详情

EQUATION

反应方程式

HRID 2163438 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 20 parts of α-phenylacetonitrile in 300 parts by volume of toluene is added 94 parts of 3-(2-chloroethyl)-3-azabicyclo[3.2.2]nonane dissolved in 500 parts by volume of toluene. The mixture is heated with stirring to about 80° C. and then 17 parts of sodium amide is added slowly over a period of 30 minutes. The mixture is heated at 80° C. for another 30 minutes and then cooled to room temperature. 500 Parts by volume of water is then added to the mixture and the organic layer separated and extracted with dilute hydrochloric acid. The aqueous acidic extract is made alkaline by the addition of dilute sodium hydroxide. The alkaline mixture is extracted with ether, the ether extract dried over calcium sulfate and distilled to afford 2-phenyl-4-(3-azabicyclo[3.2.2]non-3-yl)butyronitrile.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureThe mixture is heated at 80° C. for another 30 minutes
  3. temperaturecooled to room temperature
  4. customthe organic layer separated
  5. extractionextracted with dilute hydrochloric acid
  6. extractionThe aqueous acidic extract
  7. additionby the addition of dilute sodium hydroxide
  8. extractionThe alkaline mixture is extracted with ether
  9. extractionthe ether extract
  10. dry with materialdried over calcium sulfate
  11. distillationdistilled