反应详情

A solution of 1.075 g of 7-chloro-5-phenyl-1,3-dihydro-2H-1-benzazepin-2-one in 20 ml of dry tetrahydrofuran is treated with 0.23 g of sodium hydride (50% dispersion in mineral oil) and stirred at 60° for 1 hour. The mixture is then cooled to room temperature, treated with 1.53 g of bis-(4-morpholinyl)phosphinic acid chloride and stirred at this temperature for a further 2 hours. A solution of 0.593 g of acetic acid hydrazide in 50 ml of n-butanol is subsequently added thereto, the mixture is heated to boiling under reflux for 1 hour and then evaporated in vacuo. The residue is partitioned between water and methylene chloride. The methylene chloride solution is evaporated and the residue is chromatographed on 100 g of aluminium oxide (activity grade III). Various impurities and starting material are eluted successively with benzene and ethyl acetate/hexane (1:1). After elution with chloroform/ethanol (96:4) and recrystallization of the crude product from ethyl acetate/benzene/n-hexane, there is obtained 8-chloro-1-methyl-6-phenyl-4H-s-triazolo[4,3-a][1]benzazepine of melting point 235°.

1. stirringstirred at this temperature for a further 2 hours
2. temperaturethe mixture is heated
3. temperatureunder reflux for 1 hour
4. customevaporated in vacuo
5. customThe residue is partitioned between water and methylene chloride
6. customThe methylene chloride solution is evaporated
7. customthe residue is chromatographed on 100 g of aluminium oxide (activity grade III)
8. washare eluted successively with benzene and ethyl acetate/hexane (1:1)
9. washAfter elution
10. customwith chloroform/ethanol (96:4) and recrystallization of the crude product from ethyl acetate/benzene/n-hexane