反应详情

A suspension of 1-acetylpiperazine (0.627 g), 2-chloro-4′-fluoroacetophenone (0.844 g), and potassium hydrogen carbonate (0.735 g) in acetonitrile (12 ml) was stirred at ambient temperature for 3 days. After removal of the solid by filtration, the filtrate was evaporated under reduced pressure to give a residue, which was chromatographed on silica gel (100 ml) eluting with 0%-5% methanol in dichloromethane. The objective compound of the free form was taken up into ethyl acetate (2 ml) and to the solution was added a solution of hydrogen chloride in ethyl acetate (4N, 2 ml). The resulting precipitate was collected by filtration, washed with diisopropyl ether, and dried in vacuo to give 1-acetyl-4-(4-fluorophenylcarbonylmethyl)-piperazine hydrochloride (1.47 g).

1. customAfter removal of the solid
2. filtrationby filtration
3. customthe filtrate was evaporated under reduced pressure
4. customto give a residue, which
5. customwas chromatographed on silica gel (100 ml)
6. washeluting with 0%-5% methanol in dichloromethane
7. additionwas added a solution of hydrogen chloride in ethyl acetate (4N, 2 ml)
8. filtrationThe resulting precipitate was collected by filtration
9. washwashed with diisopropyl ether
10. customdried in vacuo