반응 #1451444

반응 방정식

3-(4-Benzo[b]thiophen-4-yl-piperazin-1-yl)propan-1-ol

carbon tetrachloride

triphenyl phosphine

methanol

→

1-benzo[b]thiophen-4-yl-4-(3-chloropropyl)piperazine

용매

methylene chloride

methylene chloride

반응 조건

후처리

1. 1
   온도under reflux for 3 hours
2. 2
   workup.ADDITIONSilica gel (30 g) was added to the uniform solution
3. 3
   기타the solvent was evaporated under reduced pressure
4. 4
   기타The residue was purified by silica gel column chromatography (silica gel: 300 g, n-hexane:ethyl acetate=2:1)
5. 5
   농축concentrated under reduced pressure

실험 절차

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 methylene chloride, and carbon tetrachloride (30 ml) and triphenyl phosphine (4.06 g, 15.5 mmol) were added thereto followed by stirring under reflux for 3 hours. The reaction mixture was cooled to room temperature, then methanol and methylene chloride were added thereto so as to make the mixture uniform. Silica gel (30 g) was added to the uniform solution, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (silica gel: 300 g, n-hexane:ethyl acetate=2:1), then concentrated under reduced pressure to obtain 1-benzo[b]thiophen-4-yl-4-(3-chloropropyl)piperazine (2.36 g) as colorless oil.

출처