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

HRID 5090

反応式

HRID 5090 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 57243155HCID 57243155、化合物

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-3f825583ac204effbee8944eb1dc37d3
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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