反应详情

温度

100 °C

A mixture of 1-(4-pyridyl)piperazine (0.86 g), N-methyl-4-fluorobenzenesulphonamide (1.00 g) and potassium carbonate (2.00 g) in N-methylpyrrolidone was stirred at 100° C. for 24 hours and then evaporated. The residue was partitioned between dichloromethane and 2N hydrochloric acid. The acid layer was washed with dichloromethane, filtered and made basic with sodium bicarbonate solution. The mixture was extracted several times with chloroform, and the combined extracts were washed with water, dried over magnesium sulphate and evaporated. The residue was crystallised from ethanol/ethyl acetate to give the title compound (0.12 g), m.p. 204°-206° C. Found: C,57.55; H,6.13; N,16.62. C16H20N4O2S requires: C,57.81; H,6.06; N,16.85%.

1. customevaporated
2. customThe residue was partitioned between dichloromethane and 2N hydrochloric acid
3. washThe acid layer was washed with dichloromethane
4. filtrationfiltered
5. extractionThe mixture was extracted several times with chloroform
6. washthe combined extracts were washed with water
7. dry with materialdried over magnesium sulphate
8. customevaporated
9. customThe residue was crystallised from ethanol/ethyl acetate