反应详情

To 10-methyl-2,3-dihydro-1H-pyrrolo[2,1-c][1,4]benzodiazapine-5,11(10H, 11aH)-dione (5.7 g, 24.7 mmol) in concentrated sulfuric acid (60 ml) at 0° C. was added potassium nitrate (2.62 g, 25.9 mmol). After stirring for 2 h the mixture was dumped onto ice (500 g) and extracted with ethyl acetate (5×75 ml). The combined extracts were washed with water, dried over magnesium sulfate, filtered, and concentrated to a solid which was recrystallized from ethyl acetate-hexane (5.2 g, 77%), m.p. 160-162° C.

1. extractionextracted with ethyl acetate (5×75 ml)
2. washThe combined extracts were washed with water
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated to a solid which
6. customwas recrystallized from ethyl acetate-hexane (5.2 g, 77%), m.p. 160-162° C.