Dichloromethane → HCID 178459483, compound

Participants

Reaction Steps

To a solution of 7-chloro-3-(carboxy)pyrazolo[3,4-c][1]-benzazepine-4,10(1H,9H)-dione (500 mg, 1.7 mmol) (compound of Example 9) in dichloromethane (15 mL) was added N,N-dimethylformamide (2 drops) and then in one portion oxalyl chloride (300 μL, 3.4 mmol). The resulting solution was stirred for 24 hours at room temperature, concentrated by rotary evaporation, and allyl alcohol (15 mL) was added to the residue. The mixture was heated at 100° C. for 15 minutes and concentrated by rotary evaporation. The residue was purified by flash chromatography eluting with dichloromethane:methanol (95:5) to give the title compound as a solid (358 mg, 63% yield, 247-249° C.).

Provenance & Evidence