反应 #66588

反应方程式

Acetic acid trifluoroacetic acid

2-(3,4-dimethoxyphenyl)ethanamine

hexamethylenetetramine

→

title product

收率 95.0%

6,7-Dimethoxy-3,4-dihydroisoquinoline

收率 95.0%

溶剂

water

反应条件

后处理

1. 1
   温度The resulting solution was heated
2. 2
   温度at reflux for about 5 hours in an oil bath
3. 3
   萃取the solution was extracted with dichloromethane (3×200 mL)
4. 4
   干燥dried over anhydrous sodium sulfate
5. 5
   其他Solids were removed by filtration
6. 6
   浓缩the resulting filtrate was concentrated in vacuo

实验过程

Acetic acid/trifluoroacetic acid (100 mL) was added to a solution of 2-(3,4-dimethoxyphenyl)ethanamine (20 g, 110.38 mmol, 1.00 equiv) and hexamethylenetetramine (31 g, 221.11 mmol, 2.00 equiv). The resulting solution was heated at reflux for about 5 hours in an oil bath. After adding water (100 mL), the solution was extracted with dichloromethane (3×200 mL), and the organic layers were combined and dried over anhydrous sodium sulfate. Solids were removed by filtration, and the resulting filtrate was concentrated in vacuo to give the title product as a yellow oil (20 g, yield=95%). LC-MS: m/z=192 (MH)+.

来源