反応 #156240

反応方程式

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

溶媒

DMF

ethyl acetate

反応条件

後処理

1. 1
   その他After the reaction liquid
2. 2
   その他condensed under reduced pressure
3. 3
   その他the residue was purified by silica gel column chromatography (ethyl acetate:methanol=95:5→60:40)
4. 4
   その他condensed under reduced pressure
5. 5
   その他The generated insoluble matter was separated by filtration
6. 6
   その他dried

実験手順

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.

出典