Methyl fluorosulfate → (2S, 4S)-1,1-Dimethyl-2-methylcarbamoyl-4-(4-methoxybenzylthio)pyrrolidinium fluorosulfate

HRID 5076

반응식

HRID 5076 반응식
[F:1][S:2]([O:5][CH3:6])(=[O:4])=[O:3].[CH3:7][O:8][C:9]1[CH:26]=[CH:25][C:12]([CH2:13][S:14][C@@H:15]2[CH2:19][N:18]([CH3:20])[C@H:17]([C:21](=[O:24])[NH:22][CH3:23])[CH2:16]2)=[CH:11][CH:10]=1>C(Cl)Cl>[S:2]([F:1])([O-:5])(=[O:4])=[O:3].[CH3:20][N+:18]1([CH3:6])[CH2:19][C@@H:15]([S:14][CH2:13][C:12]2[CH:11]=[CH:10][C:9]([O:8][CH3:7])=[CH:26][CH:25]=2)[CH2:16][C@H:17]1[C:21](=[O:24])[NH:22][CH3:23]

참가 물질

4

반응물 2

HCID 9870Methyl fluorosulfateHCID 14880279(2S, 4S)-4-(4-Methoxybenzylthio)-1-methyl-2-methylcarbamoylpyrrolidine

생성물 1

HCID 86747188(2S, 4S)-1,1-Dimethyl-2-methylcarbamoyl-4-(4-methoxybenzylthio)pyrrolidinium fluorosulfate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

280 μl of methyl fluorosulfonate were added, whilst ice-cooling, to a solution of 210 mg of (2S, 4S)-4-(4-methoxybenzylthio)-1-methyl-2-methylcarbamoylpyrrolidine [prepared as described in step (5) above] dissolved in 30 ml of dry methylene chloride. The mixture was stirred at the same temperature for 30 minutes and then at room temperature for 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 reduced rpessure, to afford 281 mg of the title compound as a colorless powder.

후처리

  1. waitat room temperature for 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-1d2785f1e38445e281416d2d2b06b4b3
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05242914

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