反应详情

温度

60 °C

Iron powder (56 mg, 1 mmol) was added to a mixture of (R)-5-(1,4-dimethyl-6-(6-nitropyridin-3-yl)-5,6-dihydro-4H-benzo[b][1,2,4]triazolo[4,3-d][1,4]diazepin-8-yl)pyridin-2-amine (86 mg, 0.2 mmol) in a mixed solvents of ammonium chloride aqueous (2 mL) and ethanol (10 mL). Once addition was complete, the mixture was heated to 60° C. for 2 hours. The mixture was filtered. The filtrate was concentrated, diluted with water (10 mL), extracted with ethyl acetate (20 mL×2). The combined organic layers were dried over anhydrous sodium sulfate, filtered and concentrated to give a residue which was purified by column chromatography (silica gel, dichloromethane/methanol=8:1) to afford (R)-5,5′-(1,4-dimethyl-4H-benzo[b][1,2,4]triazolo[4,3-d][1,4]diazepine-6,8(5H)-diyl)dipyridin-2-amine (8 mg, 20%).

1. additionOnce addition
2. filtrationThe mixture was filtered
3. concentrationThe filtrate was concentrated
4. additiondiluted with water (10 mL)
5. extractionextracted with ethyl acetate (20 mL×2)
6. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customto give a residue which
10. customwas purified by column chromatography (silica gel, dichloromethane/methanol=8:1)