HRID2237462

反应详情

EQUATION

反应方程式

HRID 2237462 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 solution of 2-nitrobenzyl amine (17 g, 78 mmol) in DMF (50 mL) was cooled to 0° C. and treated dropwise with a solution of 3-amino-1-propanol (50 mL, 0.65 mol) in DMF (150 mL) over 0.5 hours. The reaction mixture was stirred at 0° C. for 1 hour, then warmed to room temperature for 2 hours, and evaporated to a red oil. The crude product residue was purified by flash chromatography (SiO2, 10% 0.5 M NH3-methanol/dichloromethane) to afford 3-[(2-nitrobenzyl)amino]propan-1-ol (16 g, 98%) as a yellow oil:

WORKUP

后处理

  1. temperaturewarmed to room temperature for 2 hours
  2. customevaporated to a red oil
  3. customThe crude product residue was purified by flash chromatography (SiO2, 10% 0.5 M NH3-methanol/dichloromethane)