HRID359994

反应详情

EQUATION

反应方程式

HRID 359994 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 15 g of lithium aluminum hydride in 200 ml of anhydrous ethyl ether under argon was added, at room temperature, a solution of 32.0 g of 4-butylbenzamide in 200 ml of freshly distilled tetrahydrofuran. The resulting mixture was stirred at room temperature for one hour and then heated at reflux for 20 hours. The mixture was cooled and sodium sulfate decahydrate was cautiously added portionwise to the mixture until it was colorless. The mixture was stirred for 30 minutes. The mixture was filtered and the filter was washed with ether. The filtrate was evaporated in vacuo to yield 29 g (99% yield) of a liquid. The liquid was distilled by Kugelrohr distillation, bp 85° C./0.070 mm of mercury, to give the desired product as a colorless liquid.

WORKUP

后处理

  1. additionwas added, at room temperature
  2. temperatureheated
  3. temperatureat reflux for 20 hours
  4. temperatureThe mixture was cooled
  5. stirringThe mixture was stirred for 30 minutes
  6. filtrationThe mixture was filtered
  7. washthe filter was washed with ether
  8. customThe filtrate was evaporated in vacuo