반응 #1281600

반응 방정식

1-amino-2-methylimidazole hydrochloride

p-(dimethylamino)benzaldehyde

→

1-[[p-(dimethylamino)benzylidene]amino]-2-methylimidazole

용매

acetic acid

반응 조건

후처리

1. 1
   기타The mixture is evaporated, whereupon the residue
2. 2
   workup.ADDITIONis treated four times with ethanol
3. 3
   기타again evaporated each time
4. 4
   세척The crystalline residue is washed with ether
5. 5
   workup.ADDITIONtreated with saturated sodium hydrogen carbonate solution
6. 6
   추출The mixture is extracted with methylene chloride
7. 7
   건조the extract is dried over sodium sulfate
8. 8
   기타evaporated
9. 9
   기타the material obtained
10. 10
    기타is recrystallized from methylene chloride/petroleum ether

실험 절차

1.3 g of 1-amino-2-methylimidazole hydrochloride and 2.2 g of p-(dimethylamino)benzaldehyde are stirred at room temperature for 16 hours in 100 ml of glacial acetic acid. The mixture is evaporated, whereupon the residue is treated four times with ethanol and again evaporated each time. The crystalline residue is washed with ether and then treated with saturated sodium hydrogen carbonate solution. The mixture is extracted with methylene chloride, the extract is dried over sodium sulfate and evaporated, and the material obtained is recrystallized from methylene chloride/petroleum ether. There is obtained 1-[[p-(dimethylamino)benzylidene]amino]-2-methylimidazole of melting point 166°-167°.

출처