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Methyl fluorosulfate → (2S, 4S)-2-Ethylcarbamoyl-1-ethyl-1-methyl-4-(4-methoxybenzylthio)pyrrolidinium fluorosulfonate

HRID 5103
ノート
印刷プレビュー

反応式

HRID 5103 の反応式
[F:1][S:2]([O:5][CH3:6])(=[O:4])=[O:3].[CH2:7]([NH:9][C:10]([C@@H:12]1[CH2:16][C@H:15]([S:17][CH2:18][C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=2)[CH2:14][N:13]1[CH2:27][CH3:28])=[O:11])[CH3:8]>C(Cl)Cl>[F:1][S:2]([O-:5])(=[O:4])=[O:3].[CH2:7]([NH:9][C:10]([C@@H:12]1[CH2:16][C@H:15]([S:17][CH2:18][C:19]2[CH:20]=[CH:21][C:22]([O:25][CH3:26])=[CH:23][CH:24]=2)[CH2:14][N+:13]1([CH2:27][CH3:28])[CH3:6])=[O:11])[CH3:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 9870Methyl fluorosulfateHCID 14880288(2S, 4S)-2-Ethylcarbamoyl-1-ethyl-4-(4-methoxybenzylthio)pyrrolidine

生成物 1

HCID 86745658(2S, 4S)-2-Ethylcarbamoyl-1-ethyl-1-methyl-4-(4-methoxybenzylthio)pyrrolidinium fluorosulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

233 μl of methyl fluorosulfonate were added, whilst ice-cooling, to a solution of 910 mg of (2S, 4S)-2-ethylcarbamoyl-1-ethyl-4-(4-methoxybenzylthio)pyrrolidine dissolved in 35 ml of dry methylene chloride, and the mixture was stirred 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 washed by decantation with diethyl ether and dried under reduced pressure, to afford 1.20 g of the title compound as a pale brown oil.

後処理

  1. customAt the end of this time, the solvent was removed by distillation under reduced pressure
  2. washthe residue was washed by decantation with diethyl ether
  3. customdried under reduced pressure

出典と根拠

ORDレコード
ord-a8f8a3b32f32483890fe4ab467777b15
出典データセット
uspto-grants-1993_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05242914

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート