反应 #302877
ord-3f10e5be0a554b0ebb6dca4b45a5880d
反应方程式
2-aminobenzimidazole
ethyl acrylate
→
3,4-dihydro-pyrimidino[1,2-a]benzimidazol-2(1H)-one
收率 54.7%
反应条件
温度
130°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度to cool down to room temperature
- 2workup.WAITUpon standing over night
- 3其他3,4-dihydro-pyrimidino[1,2-a]benzimidazol-2(1H)-one crystallized from the medium
- 4其他was isolated by filtration
- 5其他3,4-dihydro-pyrimidino[1,2-a]benzimidazol-2(1H)-one was recrystallized from 1-methoxy-2-propanol
实验过程
5.32 g (40 mmol) 2-aminobenzimidazole and 4.00 (40 mmol) ethyl acrylate were dissolved in 25 ml Proglyde DMM. The reaction mixture was heated to 130° C. and the reaction was allowed to continue for 6 hours at 130° C. The reaction mixture was allowed to cool down to room temperature. Upon standing over night, 3,4-dihydro-pyrimidino[1,2-a]benzimidazol-2(1H)-one crystallized from the medium and was isolated by filtration. 3,4-dihydro-pyrimidino[1,2-a]benzimidazol-2(1H)-one was recrystallized from 1-methoxy-2-propanol. 4.1 g (54.7%) 3,4-dihydro-pyrimidino[1,2-a]benzimidazol-2(1H)-one was isolated (m.p. >260° C.).