HRID1872702

反应详情

EQUATION

反应方程式

HRID 1872702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-nitro-N-methylphthalimide (0.58 g, 2.8 mmol) in dry tetrahydrofuran (10 ml) was added dropwise to a stirred suspension of lithium aluminium hydride (0.64 g, 16.8 mmol) under argon. The mixture was stirred at room temperature for 2h and then heated under gentle reflux for 2.5h. The reaction was quenched by addition of wet diethyl ether followed by a minimum amount of water. The precipithated aluminium salts were removed by filtration. The filtrate was concentrated in vacuo to give the title compound as a brown oil (400 mg) which was used directly in the next stage (Example 31).

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder gentle reflux for 2.5h
  3. customThe reaction was quenched by addition of wet diethyl ether
  4. customThe precipithated aluminium salts were removed by filtration
  5. concentrationThe filtrate was concentrated in vacuo