Methyl fluorosulfate → (3S)-1,1-Dimethyl-3-(4-methoxybenzylthio)pyrrolidinium fluorosulfonate

HRID 5090

반응식

HRID 5090 반응식
[F:1][S:2]([O:5][CH3:6])(=[O:4])=[O:3].[CH3:7][O:8][C:9]1[CH:22]=[CH:21][C:12]([CH2:13][S:14][C@H:15]2[CH2:19][CH2:18][N:17]([CH3:20])[CH2:16]2)=[CH:11][CH:10]=1>C(Cl)Cl>[F:1][S:2]([O-:5])(=[O:4])=[O:3].[CH3:20][N+:17]1([CH3:6])[CH2:18][CH2:19][C@H:15]([S:14][CH2:13][C:12]2[CH:11]=[CH:10][C:9]([O:8][CH3:7])=[CH:22][CH:21]=2)[CH2:16]1

참가 물질

4

반응물 2

HCID 9870Methyl fluorosulfateHCID 57243155HCID 57243155, 화합물

생성물 1

HCID 10784133(3S)-1,1-Dimethyl-3-(4-methoxybenzylthio)pyrrolidinium fluorosulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

118 μl of methyl fluorosulfonate were added, whilst ice-cooling, to a solution of 340 mg of (3S)-3-(4-methoxybenzylthio)-1-methylpyrrolidine [prepared as described in step (4) above] dissolved in 20 ml of dry methylene chloride. The mixture was then stirred at the same temperature for 30 minutes and then at room temperature for 3.5 hours. At the end of this time, the solvent was removed by distillation under reduced pressure, and the residue was repeatedly washed by decantation with diethyl ether and dried under reduced pressure to afford 500 mg of the title compound as a colorless powder.

후처리

  1. waitat room temperature for 3.5 hours
  2. customAt the end of this time, the solvent was removed by distillation under reduced pressure
  3. washthe residue was repeatedly washed by decantation with diethyl ether
  4. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-3f825583ac204effbee8944eb1dc37d3
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05242914

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