反应详情

A solution of 32.4 g of phenyl chloroformate in 100 ml of acetonitrile was added dropwise under nitrogen while stirring to a mixture of 34.6 g of 2-(2-aminobenzyl)imidazole and 71 g of triethylamine in 600 ml of acetonitrile at room temperature. After addition was complete, the reaction mixture was heated under reflux for 12 hours, and allowed to cool to room temperature. Water (150 ml) was added, the mixture was stirred at room temperature for 0.5 hour and cooled to 5°. The resulting precipitate was filtered off, washed first twice with 50 ml of water, then 3 times with 33 ml of cold acetone and dried to give 11H-imidazo[1,2-c][1,3]benzodiazepin-5-(6H)-one, m.p. 225°-7°.

1. additionAfter addition
2. temperaturethe reaction mixture was heated
3. temperatureunder reflux for 12 hours
4. temperaturecooled to 5°
5. filtrationThe resulting precipitate was filtered off
6. washwashed first twice with 50 ml of water
7. dry with material3 times with 33 ml of cold acetone and dried