HRID261204

反应详情

EQUATION

反应方程式

HRID 261204 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

252 g of 3-[N-(p-chlorocinnamyl)-methylamino]propionitrile in 1 liter of hexamethylphosphoric acid triamide (HMPT) are added dropwise over a period of 11/4 hours at 0°-5° and in a nitrogen atmosphere to a suspension of 36 g of sodium hydride (80% in mineral oil) in 2 liter of HMPT, and the mixture stirred at room temperature for a period of 16 hours. Water is then added to the mixture with ice cooling, the mixture extracted with ether, the organic phase washed with water, dried over sodium sulphate and evaporated to yield 4-(p-chlorobenzyl)-1-methylpyrrolidin-3-carbonitrile. M.P. 170°-172° [hydrogen oxalate form].

WORKUP

后处理

  1. extractionthe mixture extracted with ether
  2. washthe organic phase washed with water
  3. dry with materialdried over sodium sulphate
  4. customevaporated