反应详情

A solution of N-(3-{2-[4-(2-methyl-5-quinolinyl)-1-piperazinyl]ethyl}phenyl)acetamide (50 mg) was dissolved in THF (2.5 mL) and sodium hydride (60% w/w oil dispersion, 0.005 g, 1 eq.) was added at 0° C. After 5 minutes iodomethane was added (5 uL, 1.0 eq.) and the mixture was warmed to room temperature. After 10 h the solution was partitioned between water (3 mL) and ethyl acetate (3×5 mL). The combined organic extracts were washed with brine, dried over sodium sulfate and concentrated under vacuum. The crude was purified by flash chromatography on silica gel, eluting with a gradient from dichloromethane to dichloromethane-methanol (98:2) affording the title compound in 61% yield (0.02 g).

1. customAfter 10 h the solution was partitioned between water (3 mL) and ethyl acetate (3×5 mL)
2. washThe combined organic extracts were washed with brine
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated under vacuum
5. customThe crude was purified by flash chromatography on silica gel
6. washeluting with a gradient from dichloromethane to dichloromethane-methanol (98:2)