반응 #4393

반응 방정식

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

formaldehyde

dimethylamine

→

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

수율 85.4%

용매

acetic acid

반응 조건

후처리

1. 1
   온도cooling over a period of 10 minutes
2. 2
   온도The mixture was heated at 50°-55° C. for 2 hours
3. 3
   기타evaporated in vacuo
4. 4
   추출extracted with methylene chloride
5. 5
   세척The extract was washed with water
6. 6
   건조dried over magnesium sulfate
7. 7
   기타evaporated in vacuo
8. 8
   기타The residual solid was recrystallized from a mixture of diethyl ether and n-hexane

실험 절차

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).

출처