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Trifluoroacetic acid → 3-Mercapto-2-pyrrolidinone trifluoromethanesulfonate

HRID 5118
ノート
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反応式

HRID 5118 の反応式
FC(F)(F)C(O)=O.[F:8][C:9]([F:15])([F:14])[S:10]([OH:13])(=[O:12])=[O:11].COC1C=CC(C[S:23][CH:24]2[CH2:28][CH2:27][NH:26][C:25]2=[O:29])=CC=1>C1(OC)C=CC=CC=1>[F:8][C:9]([F:15])([F:14])[S:10]([OH:13])(=[O:12])=[O:11].[SH:23][CH:24]1[CH2:28][CH2:27][NH:26][C:25]1=[O:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 62406Trifluoromethanesulfonic acidHCID 102432413-(4-Methoxybenzylthio)pyrrolidin-2-one

生成物 1

HCID 197972633-Mercapto-2-pyrrolidinone trifluoromethanesulfonate

試薬・触媒・溶媒 1

HCID 7519Anisole溶媒

実験手順

20 ml of trifluoroacetic acid and 0.41 ml of trifluoromethanesulfonic acid were added, whilst ice-cooling, to a solution of 949 mg of 3-(4-methoxybenzylthio)pyrrolidin-2-one in 4 ml of anisole, and then the mixture was stirred at room temperature for 30 minutes. At the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure to leave a residue, which was purified by column chromatography through silica gel, eluted with a 10:1 by volume mixture of ethyl acetate and methanol, to give 728 mg of the title compound as an oil.

後処理

  1. concentrationAt the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure
  2. customto leave a residue, which
  3. customwas purified by column chromatography through silica gel
  4. washeluted with a 10:1 by volume mixture of ethyl acetate and methanol

出典と根拠

ORDレコード
ord-715795a169ab49eca88ae924fb7a34b7
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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