反应 #811394

反应方程式

3-Bromo-1-(1H-imidazol-4-yl)-1-propanone

triethylamine

Triethylamine

→

title compound

收率 38.9%

5,6-dihydro-7H-pyrrolo[1,2-c]imidazol-7-one

收率 38.9%

溶剂

acetonitrile

acetonitrile

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture was stirred for 30 min
2. 2
   温度The reaction mixture was cooled to room temperature
3. 3
   过滤the insoluble material was filtered off
4. 4
   其他The solvent was evaporated
5. 5
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate again
6. 6
   过滤The insoluble material was filtered off
7. 7
   其他the solvent was evaporated
8. 8
   workup.ADDITIONThe resulting residue was subjected to silica gel column chromatography (eluent; dichloromethane:methanol containing ammonia (5%)=10:1) for purification

实验过程

3-Bromo-1-(1H-imidazol-4-yl)-1-propanone (28.5 g) was suspended in acetonitrile (1100 ml) and the suspension was warmed to 70° C. A solution of triethylamine (15.3 ml) in acetonitrile (25 ml) was slowly added dropwise and the mixture was stirred at 70° C. for 2 h. Triethylamine (25 ml) was further added and the mixture was stirred for 30 min. The reaction mixture was cooled to room temperature and the insoluble material was filtered off. The solvent was evaporated and the residue was dissolved in ethyl acetate again. The insoluble material was filtered off and the solvent was evaporated. The resulting residue was subjected to silica gel column chromatography (eluent; dichloromethane:methanol containing ammonia (5%)=10:1) for purification to give the title compound (6.67 g) as a colorless powder.

来源