Methyl fluorosulfate → 1,1-Dimethyl-4-(4-methoxybenzylthio)piperidinium fluorosulfonate

HRID 1030153

Reaktionsgleichung

Reaktionsgleichung von HRID 1030153
[F:1][S:2]([O:5][CH3:6])(=[O:4])=[O:3].[CH3:7][O:8][C:9]1[CH:23]=[CH:22][C:12]([CH2:13][S:14][CH:15]2[CH2:20][CH2:19][N:18]([CH3:21])[CH2:17][CH2:16]2)=[CH:11][CH:10]=1>C(Cl)Cl>[F:1][S:2]([O-:5])(=[O:4])=[O:3].[CH3:21][N+:18]1([CH3:6])[CH2:17][CH2:16][CH:15]([S:14][CH2:13][C:12]2[CH:11]=[CH:10][C:9]([O:8][CH3:7])=[CH:23][CH:22]=2)[CH2:20][CH2:19]1

Komponenten

4

Edukt 2

HCID 9870Methyl fluorosulfateHCID 197972594-(4-Methoxybenzylthio)-1-methylpiperidine

Produkt 1

HCID 867456551,1-Dimethyl-4-(4-methoxybenzylthio)piperidinium fluorosulfonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

2.9 ml of methyl fluorosulfonate were added, whilst ice-cooling, to a solution of 8.95 g of 4-(4-methoxybenzylthio)-1-methylpiperidine dissolved in 300 ml of dry methylene chloride, and the mixture was stirred at the same temperature for 20 minutes and then at room temperature for 2.5 hours. At the end of this time, the solvent was removed by distillation under reduced pressure, and the residue was washed repeatedly by decantation with diethyl ether and dried under reduce pressure, to afford 12.76 g of the title compound as a colorless powder.

Aufarbeitung

  1. waitat room temperature for 2.5 hours
  2. customAt the end of this time, the solvent was removed by distillation under reduced pressure
  3. washthe residue was washed repeatedly by decantation with diethyl ether
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-15335184219c46c7afe47f1040f3a8f4
Quelldatensatz
uspto-grants-1992_04
Patentnummer
US05104867

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