反应详情

温度

120 °C

To a mixture of 5-chloro-2-pyridinyl phenyl sulfone (10.2 g, 40.2 mmol) in pyridine (100 mL) was added piperazine (13.8 g, 161 mmol). The mixture was heated to 120° C. in a preheated oil bath for 18 h. The mixture then was removed from heat and cooled to room temperature. The mixture was partitioned between water and ethyl acetate. The layers were separated and the organic layer washed twice with water (2×50 mL). The organic layer was dried with anhydrous magnesium sulfate and concentrated. The solids obtained after concentration were recrystallized from water and dried to give 5.89 g of the title compound; m.p. 126-127° C.; IR (drift) 1568, 1479, 1447, 1306, 1290, 1254, 1175, 1154, 1145, 1104, 830, 756, 715, 688, 602 cm−1. 1H NMR (CDCl3) δ 3.0, 3.29, 7.13, 7.53, 8.01, 8.26.

1. customThe mixture then was removed
2. temperaturefrom heat
3. temperaturecooled to room temperature
4. customThe mixture was partitioned between water and ethyl acetate
5. customThe layers were separated
6. washthe organic layer washed twice with water (2×50 mL)
7. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
8. concentrationconcentrated
9. customThe solids obtained
10. concentrationafter concentration
11. customwere recrystallized from water
12. customdried