反应详情

A DMF solution(4 ml) of 5-(2,2-dihydroxyethyl)-2-methyl-5H-furo[3,2-c]pyridine-4-one(0.20 g), 7-[3-(3-aminopyridin-4-ylamino)propoxy]-1-ethyl-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione(0.37 g), and sodium hydrogensulfite(0.47 g) were heated at 180° C. for 10 minutes (microwave reactor). After the reaction liquid was condensed under reduced pressure, the residue was purified by silica gel column chromatography (ethyl acetate: methanol=95:5→60:40). The purified product was condensed under reduced pressure. A 4N-hydrogen chloride ethyl acetate solution was added to an ethyl acetate solution of the residue, which was stirred at room temperature. The generated insoluble matter was separated by filtration, and dried to give the title compound(0.47 g) as a white amorphous solid.

1. customAfter the reaction liquid
2. customcondensed under reduced pressure
3. customthe residue was purified by silica gel column chromatography (ethyl acetate: methanol=95:5→60:40)
4. customcondensed under reduced pressure
5. customThe generated insoluble matter was separated by filtration
6. customdried