反应详情

A stirred mixture of 5.2 g of 4-amino-5-imidazolecarboxamide hydrochloride and 10.0 g of 2',5'-dichloro-3-dimethylaminoacrylophenone (prepared as described in Example 4) in 80 ml of glacial acetic acid was heated at reflux for 4 hours. Evaporation in vacuo gave a dark oil which was dissolved in dichloromethane and treated with saturated sodium bicarbonate. The organic layer was separated, washed with water then dried over anhydrous sodium sulfate. The dichloromethane solution was passed through a short column of hydrous magnesium silicate. Evaporation of the eluate gave a semi-solid which was treated with hot dichloromethane-hexane to give a yellow precipitate which was collected by filtration and dried to give 7.3 g of the product of the example, mp 230°-234° C.

1. temperaturewas heated
2. temperatureat reflux for 4 hours
3. customEvaporation in vacuo
4. customgave a dark oil which
5. customThe organic layer was separated
6. washwashed with water
7. dry with materialthen dried over anhydrous sodium sulfate
8. customEvaporation of the eluate
9. customgave a semi-solid which
10. customto give a yellow precipitate which
11. filtrationwas collected by filtration
12. customdried