反应详情

温度

90 °C

A mixture consisting of 4.5 gm of 6,11-dihydro-2,6-dimethyl-5H-pyrido-[2,3-b][1,5]benzodiazepin-5-one, 60 ml of dioxane and 1.27 gm of 50% sodium hydride in mineral oil was stirred at 90° C. for 1 hour. Thereafter, 4.3 gm of 3-(N-ethyl-N-isopropyl-amino)-propyl chloride were added dropwise, and the mixture was refluxed for 17 hours. The reaction solution was then evaporated in vacuo, and the residue was purified over a silica gel column and recrystallized from petroleum ether, yielding 36% of theory of the compound named in the heading, which had a melting point of 104°-105° C.

1. temperaturethe mixture was refluxed for 17 hours
2. customThe reaction solution was then evaporated in vacuo
3. customthe residue was purified over a silica gel column
4. customrecrystallized from petroleum ether
5. customyielding 36% of theory of the compound