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

HRID 5076

反応式

HRID 5076 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1d2785f1e38445e281416d2d2b06b4b3
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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