反应详情

Bis-(2-methoxyethyl)amine (560 μL, 3.13 mmol) was added to a solution of trimethylaluminum in toluene (1.56 mL, 3.13 mmol) and the solution was stirred for 20 minutes. A portion (403 μL) of the resulting solution was added to a solution of 7-chloro-3-(ethoxycarbonyl)pyrazolo[3,4-c][1]benzazepine-4,10(1H,9H)-dione (100 mg, 0.313 mmol) in toluene (780 μL). The resulting solution was stirred for 24 hours at room temperature and then quenched with an aqueous hydrochloric acid solution (1.8 mL, 1N) and water (15 mL). The aqueous layer was extracted with chloroform (7×25 mL). The organic layers were combined and concentrated on a rotary evaporator. The crude product was purified by flash chromatography eluting with chloroform:2-propanol (99:1-95:5) to give the title compound (421 mg, 67% yield, m.p. 207-209° C.).

1. stirringThe resulting solution was stirred for 24 hours at room temperature
2. customquenched with an aqueous hydrochloric acid solution (1.8 mL, 1N) and water (15 mL)
3. extractionThe aqueous layer was extracted with chloroform (7×25 mL)
4. concentrationconcentrated on a rotary evaporator
5. customThe crude product was purified by flash chromatography
6. washeluting with chloroform:2-propanol (99:1-95:5)