Methyl fluorosulfate → (2S, 4S)-2-(N,N-Dimethylcarbamoyl)-4-(4-methoxybenzylthio)-1,1-dimethylpyrrolidinium fluorosulfonate

HRID 5086

反応式

HRID 5086 の反応式
[F:1][S:2]([O:5][CH3:6])(=[O:4])=[O:3].[CH3:7][N:8]([CH3:27])[C:9]([C@@H:11]1[CH2:15][C@H:14]([S:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=2)[CH2:13][N:12]1[CH3:26])=[O:10]>C(Cl)Cl>[F:1][S:2]([O-:5])(=[O:4])=[O:3].[CH3:7][N:8]([CH3:27])[C:9]([C@@H:11]1[CH2:15][C@H:14]([S:16][CH2:17][C:18]2[CH:19]=[CH:20][C:21]([O:24][CH3:25])=[CH:22][CH:23]=2)[CH2:13][N+:12]1([CH3:6])[CH3:26])=[O:10]

参加物

4

反応物 2

HCID 9870Methyl fluorosulfateHCID 57114883(2S, 4S)-2-(N,N-Dimethylcarbamoyl)-4-(4-methoxybenzylthio)-1-methylpyrrolidine

生成物 1

HCID 86747189(2S, 4S)-2-(N,N-Dimethylcarbamoyl)-4-(4-methoxybenzylthio)-1,1-dimethylpyrrolidinium fluorosulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

139 μl of methyl fluorosulfonate were added, whilst ice-cooling, to a solution of 190 mg of (2S, 4S)-2-(N,N-dimethylcarbamoyl)-4-(4-methoxybenzylthio)-1-methylpyrrolidine [prepared as described in step (5) or (11) above] dissolved in 3.8 ml of methylene chloride, and the mixture was stirred at room temperature for 2 hours. At the end of this time, the solvent was distilled off under reduced pressure. The residue was repeatedly washed by decantation with hexane and dried under reduced pressure, to give 356 mg of the title compound as an oil.

後処理

  1. distillationAt the end of this time, the solvent was distilled off under reduced pressure
  2. washThe residue was repeatedly washed by decantation with hexane
  3. customdried under reduced pressure

出典と根拠

ORDレコード
ord-57c4dcadfa504bd3b6a8c19ef17eb2ac
出典データセット
uspto-grants-1993_09
特許番号
US05242914

関連ノート

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