Methanol → 1-Benzo[b]thiophen-4-yl-4-(3-chloropropyl)piperazine

3.56 g (12.9 mmol) of 3-(4-benzo[b]thiophen-4-yl-piperazin-1-yl)propan-1-ol was suspended in 30 ml of dichloromethane, and carbon tetrachloride (30 ml) and triphenyl phosphine (4.06 g, 15.5 mmol) were added thereto. The mixture was refluxed with heating for 3 hours. The reaction solution was cooled to room temperature, then methanol and dichloromethane were added thereto to homogenize the mixture. Silica gel (30 g) was added to the solution, and the solvent was evaporated under reduced pressure. The obtained residue was loaded on silica gel column (300 g) and extracted with a solvent mixture of n-hexane:ethyl acetate=2:1. The extraction solution was concentrated under reduced pressure to obtain 1-benzo[b]thiophen-4-yl-4-(3-chloropropyl)piperazine (2.36 g) as colorless oil.

1. temperatureThe mixture was refluxed
2. temperaturewith heating for 3 hours
3. additionSilica gel (30 g) was added to the solution
4. customthe solvent was evaporated under reduced pressure
5. extractionextracted with a solvent mixture of n-hexane
6. concentrationThe extraction solution was concentrated under reduced pressure

ORD-Eintrag

ord-52edf86f6148474bb4651c8effb6e48a

Quelldatensatz

uspto-grants-2011_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08071600B2