反应详情

温度

100 °C

A mixture of 1-[1-(tert-butoxycarbonyl)piperidin-4-ylmethyl]-4-(chloromethanesulfonyl)-2-piperazinone (2.47 g), 5-chlorosalicylaldehyde (917 mg), potassium carbonate (810 mg) and DMF (30 ml) was stirred at 100° C. for 2 days, and the reaction solution was concentrated. To the residue was added water, and the mixture was extracted with ethyl acetate, washed with water and brine, dried and concentrated. The residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:4) to give colorless solid of 1-[1-(tert-butoxycarbonyl)piperidin-4-ylmethyl]-4-(5-chlorobenzofuran-2-sulfonyl)-2-piperazinone (272 mg).

1. concentrationthe reaction solution was concentrated
2. additionTo the residue was added water
3. extractionthe mixture was extracted with ethyl acetate
4. washwashed with water and brine
5. customdried
6. concentrationconcentrated
7. customThe residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:4)