Ammonium Acetate → HCID 136390211, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 3-oxo-4-(6-oxo-6,11-dihydro-5H-benzo[e]pyrido[3,2-b][1,4]diazepin-5-yl)butanoate (crude product from step 1, 0.36 g, 1 eq.) in acetic acid (5 mL) was added ammonium acetate (0.385 g, 20 eq. based on the amount of starting material used in step 1). The reaction was stirred at 120° C. for 2 hours. The reaction was poured onto water (25 mL) and extracted with dichloromethane (2×25 mL). The combined extracts were washed with water (1×25 mL), saturated sodium bicarbonate (25 mL), brine (1×25 mL), dried over sodium sulfate, filtered and concentrated under reduced pressure. Purification by column chromatography (10% methanol in dichloromethane) gave the methyl 2-(9H-benzo[f]imidazo[1,2-d]pyrido[2,3-b][1,4]diazepin-2-yl)acetate (0.4 g). LCMS: 307 [M+H].

Provenance & Evidence