反应 #1702075

反应方程式

sodium borohydride

2-bromo-5-methoxybenzaldehyde

cyclopropylamine

toluene

→

crude product

N-(2-bromo-5-methoxybenzyl)cyclopropanamine

溶剂

water

methanol

dichloromethane

反应条件

后处理

1. 1
   其他In a flask fitted with a Dean-Stark trap
2. 2
   温度at reflux for 4 hours
3. 3
   浓缩The solution was then concentrated
4. 4
   其他to give a yellow oil to which
5. 5
   温度The reaction mixture was cooled on icebath
6. 6
   workup.ADDITIONAfter complete addition
7. 7
   workup.STIRRINGthe reaction mixture was stirred 2 hours at room temperature

实验过程

In a flask fitted with a Dean-Stark trap was introduced 2-bromo-5-methoxybenzaldehyde (5.68 g, 26.41 mmol), cyclopropylamine (3.02 g, 52.83 mmol) and toluene (70 ml). The reaction mixture was stirred at room temperature for 1 hour and then at reflux for 4 hours. The solution was then concentrated to give a yellow oil to which was added methanol (30 ml). The reaction mixture was cooled on icebath followed by portionwise addition of sodium borohydride (2.00 g, 52.83 mmol). After complete addition, the reaction mixture was stirred 2 hours at room temperature, and then water (70 ml) was added. The crude product was isolated by extraction with dichloromethane and the combined organic phases were dried over sodium sulfate, filtered, and finally evaporated under reduced pressure.

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