反应详情

A mixture of 4.5 gm of 6,11-dihydro-6-methyl-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one, 0.83 gm of 55% sodium hydride in mineral oil, and 100 ml of absolute xylene was refluxed for two hours. Thereafter, 7 gm of p-toluenesulfonic acid 3-dimethylamino-n-propyl ester were added, and the resulting mixture was refluxed for 14 hours more. After cooling, the reaction mixture was suction-filtered, and the filtrate was extracted with dilute acetic acid. From the acidic aqueous phase, the base was precipitated as an oil with concentrated ammonia and taken up in ether. After evaporation of the ether solution, the residue was distilled, yielding 2.4 gm of 11(3'-dimethylamino-n-propyl)-6,11-dihydro-6-methyl-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one, b.p. 180°-183° C. at 0.03 mm Hg, which melted at 98.5°-100° C. after crystallization from cyclohexane and recrystallization from petroleum ether.

1. temperaturewas refluxed for two hours
2. temperaturethe resulting mixture was refluxed for 14 hours more
3. temperatureAfter cooling
4. filtrationthe reaction mixture was suction-filtered
5. extractionthe filtrate was extracted with dilute acetic acid
6. customFrom the acidic aqueous phase, the base was precipitated as an oil with concentrated ammonia
7. customAfter evaporation of the ether solution
8. distillationthe residue was distilled