Methyl fluorosulfate → 1,1-Dimethyl-4-(4-methoxybenzylthio)piperidinium fluorosulfonate

HRID 1030153ノート

反応式

HRID 1030153 の反応式
[F:1][S:2]([O:5][CH3:6])(=[O:4])=[O:3].[CH3:7][O:8][C:9]1[CH:23]=[CH:22][C:12]([CH2:13][S:14][CH:15]2[CH2:20][CH2:19][N:18]([CH3:21])[CH2:17][CH2:16]2)=[CH:11][CH:10]=1>C(Cl)Cl>[F:1][S:2]([O-:5])(=[O:4])=[O:3].[CH3:21][N+:18]1([CH3:6])[CH2:17][CH2:16][CH:15]([S:14][CH2:13][C:12]2[CH:11]=[CH:10][C:9]([O:8][CH3:7])=[CH:23][CH:22]=2)[CH2:20][CH2:19]1

参加物

4

反応物 2

HCID 9870Methyl fluorosulfateHCID 197972594-(4-Methoxybenzylthio)-1-methylpiperidine

生成物 1

HCID 867456551,1-Dimethyl-4-(4-methoxybenzylthio)piperidinium fluorosulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2.9 ml of methyl fluorosulfonate were added, whilst ice-cooling, to a solution of 8.95 g of 4-(4-methoxybenzylthio)-1-methylpiperidine dissolved in 300 ml of dry methylene chloride, and the mixture was stirred at the same temperature for 20 minutes and then at room temperature for 2.5 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 reduce pressure, to afford 12.76 g of the title compound as a colorless powder.

後処理

  1. waitat room temperature for 2.5 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-15335184219c46c7afe47f1040f3a8f4
出典データセット
uspto-grants-1992_04
特許番号
US05104867

反応ノート

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