Réaction #52152

Équation de réaction

5-chloro-2-pyridinyl phenyl sulfone

piperazine

→

title compound

Rendement 48.3%

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

Rendement 48.3%

Solvants

pyridine

Conditions de réaction

Traitement

1. 1
   AutreThe mixture then was removed
2. 2
   Températurefrom heat
3. 3
   Températurecooled to room temperature
4. 4
   AutreThe mixture was partitioned between water and ethyl acetate
5. 5
   AutreThe layers were separated
6. 6
   Lavagethe organic layer washed twice with water (2×50 mL)
7. 7
   SéchageThe organic layer was dried with anhydrous magnesium sulfate
8. 8
   Concentrationconcentrated
9. 9
   AutreThe solids obtained
10. 10
    Concentrationafter concentration
11. 11
    Autrewere recrystallized from water
12. 12
    Autredried

Mode opératoire

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.

Source