Реакция #52152

Уравнение реакции

5-chloro-2-pyridinyl phenyl sulfone

piperazine

→

title compound

Выход 48.3%

Phenyl 5-(1-piperazinyl)-2-pyridinyl Sulfone

Выход 48.3%

Растворители

pyridine

Условия реакции

Обработка

1. 1
   ДругоеThe mixture then was removed
2. 2
   Температураfrom heat
3. 3
   Температураcooled to room temperature
4. 4
   ДругоеThe mixture was partitioned between water and ethyl acetate
5. 5
   ДругоеThe layers were separated
6. 6
   Промывкаthe organic layer washed twice with water (2×50 mL)
7. 7
   СушкаThe organic layer was dried with anhydrous magnesium sulfate
8. 8
   Концентрированиеconcentrated
9. 9
   ДругоеThe solids obtained
10. 10
    Концентрированиеafter concentration
11. 11
    Другоеwere recrystallized from water
12. 12
    Другоеdried

Методика

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.

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