反应详情

A mixture of (5-{[(3,5-bis-trifluoromethyl-benzyl)-(2-methyl-2H-tetrazol-5-yl)-amino]-methyl}-1,3-dimethyl-1H-pyrazolo[3,4-b]pyridin-6-yl)-cyclopropylmethyl-amine (0.25 g, 0.45 mmol), triethylamine (0.13 g, 1.3 mmol), and cyclopropanecarbonyl chloride (0.28 g, 2.7 mmol) in THF (5 mL) was prepared in 10 mL reaction vessel and irradiated with 250 Watt microwave power, under 250 psi at 80° C. for 2 h. The vessel was cooled to RT and the reaction mixture was diluted with ethyl acetate (100 mL). The ethyl acetate layer was washed with water (3×100 mL), the organic layer was separated out, dried over sodium sulfate, and concentrated. The resulting oil was purified by column chromatography using silica gel (230-400 mesh) and eluting the column with 1% methanol in dichloromethane afforded a colorless solid (0.147 g, yield: 52.5%).

1. customwas prepared in 10 mL reaction vessel
2. customirradiated with 250 Watt microwave power, under 250 psi at 80° C. for 2 h
3. washThe ethyl acetate layer was washed with water (3×100 mL)
4. customthe organic layer was separated out
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customThe resulting oil was purified by column chromatography
8. washeluting the column with 1% methanol in dichloromethane