反应详情

A mixture of N,α-bis(4-fluorophenyl)-4-piperidinemethanamine (4.63 g, 0.0153 mol), 1-[4-(3-chloropropoxy)phenyl]-2-methyl-1-propanone (3.69 g, 0.0153 mol), and potassium carbonate (2.76 g, 0.02 mol) was heated at reflux 16 h in 350 mL 1-butanol containing sodium iodide (0.2 g). The reaction was concentrated to dryness and partitioned between chloroform and water. The chloroform layer was then extracted with 5% sodium hydroxide and dried (Na2SO4). The chloroform was removed to give a red oil. This material was subjected to flash chromatography on silica gel using 2% methanol in methylene chloride to accomplish elution. Fractions of similar purities were combined, and solvents removed to give an oil. The oil was converted to the HCl salt and recrystallized from methanol-diethyl ether to give a white solid. This solid was dried 16 h at 78° C. in vacuo. The procedure utilized here furnished 5.26 g (59%) of white crystalline product, mp 221° -223° C. (dec.).

1. temperaturewas heated
2. concentrationThe reaction was concentrated to dryness
3. custompartitioned between chloroform and water
4. extractionThe chloroform layer was then extracted with 5% sodium hydroxide
5. dry with materialdried (Na2SO4)
6. customThe chloroform was removed
7. customto give a red oil
8. washelution
9. customsolvents removed
10. customto give an oil
11. customrecrystallized from methanol-diethyl ether
12. customto give a white solid
13. customThis solid was dried 16 h at 78° C. in vacuo