HRID1285038

反应详情

EQUATION

反应方程式

HRID 1285038 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 1-liter flask equipped with a paddle stirrer, a reflux condenser capped with a nitrogen bubbler, and an addition funnel, was placed 7.50 g of 1,3-bis(2-methyl-2-cyanopropyl)benzene and 250 ml of reagent grade toluene which had been passed through acid alumina under nitrogen directly into the reaction vessel. With stirring at room temperature, 107 ml of a 25% solution of diisobutylaluminum hydride in toluene was added in 1 hr. The mixture was refluxed for 17 hrs 15 min. The mixture was then worked up as described in Example 1(b). Upon distillation of the isolated product through a small Vigreux still, there was obtained 3.51 g of 1,3-bis(2,2-dimethyl-3-aminopropyl)benzene as a colorless liquid distilling at 105° to 110°/0.05 mm.

WORKUP

后处理

  1. customIn a 1-liter flask equipped with a paddle stirrer, a reflux condenser
  2. customcapped with a nitrogen bubbler, and an addition funnel
  3. temperatureThe mixture was refluxed for 17 hrs 15 min
  4. distillationUpon distillation of the isolated product through a small Vigreux still