반응 #156240

반응 방정식

5-(2,2-dihydroxyethyl)-2-methyl-5H-furo[3,2-c]pyridine-4-one

7-[3-(3-aminopyridin-4-ylamino)propoxy]-1-ethyl-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione

sodium hydrogensulfite

hydrogen chloride ethyl acetate

→

title compound

1-ethyl-3,3,5-trimethyl-7-{3-[2-(2-methyl-4-oxo-4H-furo[3,2-c]pyridin-5-ylmethyl)imidazo[4,5-c]pyridin-1-yl]propoxy}-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione dihydrochloride

용매

DMF

ethyl acetate

반응 조건

후처리

1. 1
   기타After the reaction liquid
2. 2
   기타condensed under reduced pressure
3. 3
   기타the residue was purified by silica gel column chromatography (ethyl acetate:methanol=95:5→60:40)
4. 4
   기타condensed under reduced pressure
5. 5
   기타The generated insoluble matter was separated by filtration
6. 6
   기타dried

실험 절차

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.

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