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

HRID 1030150

反応式

HRID 1030150 の反応式
[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

参加物

4

反応物 2

HCID 9870Methyl fluorosulfateHCID 57243155(3S)-3-(4-Methoxybenzylthio)-1-methylpyrrolidine

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c70a59f79b6542418299035b6cd0fd96
出典データセット
uspto-grants-1992_04
特許番号
US05104867

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