反应 #4393

反应方程式

8-(2-chlorobenzyloxy)-2-methylimidazo[1,2-a]pyridine

formaldehyde

dimethylamine

→

8-(2-chlorobenzyloxy)-3-dimethylaminomethyl-2-methylimidazo[1,2-a]pyridine

收率 85.4%

溶剂

acetic acid

反应条件

后处理

1. 1
   温度cooling over a period of 10 minutes
2. 2
   温度The mixture was heated at 50°-55° C. for 2 hours
3. 3
   其他evaporated in vacuo
4. 4
   萃取extracted with methylene chloride
5. 5
   洗涤The extract was washed with water
6. 6
   干燥dried over magnesium sulfate
7. 7
   其他evaporated in vacuo
8. 8
   其他The residual solid was recrystallized from a mixture of diethyl ether and n-hexane

实验过程

To a solution of 37% aqueous formaldehyde (2.38 g) in acetic acid (38 ml) was added dropwise 50% aqueous dimethylamine (2.63 g) with ice-cooling over a period of 10 minutes and the mixture was stirred for an additional 10 minutes. The mixture was heated at 50°-55° C. for 2 hours after an addition of 8-(2-chlorobenzyloxy)-2-methylimidazo[1,2-a]pyridine (7.6 g) thereto and then evaporated in vacuo. The residue was basified with aqueous sodium hydroxide and extracted with methylene chloride. The extract was washed with water, dried over magnesium sulfate and evaporated in vacuo. The residual solid was recrystallized from a mixture of diethyl ether and n-hexane to give 8-(2-chlorobenzyloxy)-3-dimethylaminomethyl-2-methylimidazo[1,2-a]pyridine (7.85 g).

来源