HRID6714

反应详情

EQUATION

反应方程式

HRID 6714 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A suspension of 4-phenyl-but-3-enoic acid amide (5.0 g, 31 mmol) in 250 mL dichloromethane was cooled to 0° C. Diisobutylaluminum hydride (1 M in dichloromethane, 250 mL) was added and the resulting homogeneous mixture was allowed to slowly warm to rt. The reaction was stirred for 4 days then quenched by carefully pouring the mixture onto 200 mL of 1:1 water/methanol at 0° C. The aluminum salts were removed by filtration and washed with methanol. The combined filtrate was collected and the volatile material was removed by a rotary evaporator to give of 4-phenyl-but-3-enylamine (3.62 g, 79%) as a pale yellow oil.

WORKUP

后处理

  1. temperatureto slowly warm to rt
  2. customthen quenched
  3. additionby carefully pouring the mixture onto 200 mL of 1:1 water/methanol at 0° C
  4. customThe aluminum salts were removed by filtration
  5. washwashed with methanol
  6. customThe combined filtrate was collected
  7. customthe volatile material was removed by a rotary evaporator