反应详情

To a solution of trimethylaluminum in toluene (4.68 mL, 9.38 mmol) was added dipropylamine (1.29 mL, 9.38 mmol) and the solution was stirred for 45 hours. A portion (1.9 mL) of this solution was added to a solution of 7-chloro-3-(ethoxycarbonyl)pyrazolo[3,4-c][1]benzazepine-4,10(1H,9H)-dione (500 mg, 1.56 mmol) in toluene (2 mL). Additional toluene (7 mL) was added. The solution was stirred for 70 minutes at room temperature and then quenched with 1N hydrochloric acid (9.3 mL). The layers were separated and the aqueous layer was extracted with ethyl acetate (3×50 mL). The combined organics were washed with 1N hydrochloric acid and water (25 mL) and concentrated by rotary evaporation. The crude residue was purified by chromatography eluting with hexanes:ethyl acetate (95:5-50:50) to give the title compound (31% yield, m.p. 270° C.).

1. stirringThe solution was stirred for 70 minutes at room temperature
2. customquenched with 1N hydrochloric acid (9.3 mL)
3. customThe layers were separated
4. extractionthe aqueous layer was extracted with ethyl acetate (3×50 mL)
5. washThe combined organics were washed with 1N hydrochloric acid and water (25 mL)
6. concentrationconcentrated by rotary evaporation
7. customThe crude residue was purified by chromatography
8. washeluting with hexanes:ethyl acetate (95:5-50:50)