1-[Bis(3-chlorophenyl)methyl]piperazine → Hexane-1-sulfonamide

1-[Bis(3-chlorophenyl)methyl]piperazine (5.00 g, 15.5 mmol) and N-cyclopropyl-6-chlorohexanesulfonamide (4.15 g, 17.30 mmol) were refluxed in N-ethyldiisopropylamine (25 ml) for 7 hours. The reaction mixture was concentrated in vacuo, and water was added thereto. The mixture was extracted with chloroform. The chloroform layer was washed with water, and dried over anhydrous magnesium sulfate. Subsequently, the solvent was removed by evaporation in vacuo. The resulting crude product was purified by column chromatography on silica gel with chloroform-methanol (20:1), to give N-cyclopropyl-6-[4-[bis(3-chlorophenyl)methyl)]-1-piperazinyl]hexanesulfonamide (7.73 g) as an oil (yield based on 1-[bis(3-chlorophenyl)methyl]piperazine: 94.7%).

1. concentrationThe reaction mixture was concentrated in vacuo, and water
2. additionwas added
3. extractionThe mixture was extracted with chloroform
4. washThe chloroform layer was washed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. customSubsequently, the solvent was removed by evaporation in vacuo
7. customThe resulting crude product was purified by column chromatography on silica gel with chloroform-methanol (20:1)
8. customto give N-cyclopropyl-6-[4-[bis(3-chlorophenyl)methyl)]-1-piperazinyl]

ORD-Eintrag

ord-334612ed2ecd496d86d9e62ab4ad326f

Quelldatensatz

uspto-grants-2001_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06172228B2