Reaktion #52152

Reaktionsgleichung

5-chloro-2-pyridinyl phenyl sulfone

piperazine

→

title compound

Ausbeute 48.3%

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

Ausbeute 48.3%

Lösungsmittel

pyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe mixture then was removed
2. 2
   Temperaturfrom heat
3. 3
   Temperaturcooled to room temperature
4. 4
   SonstigeThe mixture was partitioned between water and ethyl acetate
5. 5
   SonstigeThe layers were separated
6. 6
   Waschenthe organic layer washed twice with water (2×50 mL)
7. 7
   TrocknenThe organic layer was dried with anhydrous magnesium sulfate
8. 8
   Einengenconcentrated
9. 9
   SonstigeThe solids obtained
10. 10
    Einengenafter concentration
11. 11
    Sonstigewere recrystallized from water
12. 12
    Sonstigedried

Vorschrift

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.

Quelle