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

HRID 1030153

반응식

HRID 1030153 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-15335184219c46c7afe47f1040f3a8f4
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05104867

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