Trifluoroacetic acid → (2S, 4S)-4-Mercapto-2-(1-methyl-2-pyrrolidinylethylcarbamoyl)-1-(4-nitrobenzyloxycarbonyl)pyrrolidine bis(trifluoromethanesulfonate)

HRID 1033668

反応式

HRID 1033668 の反応式
COC1C=CC(C[S:8][C@@H:9]2[CH2:13][N:12]([C:14]([O:16][CH2:17][C:18]3[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][CH:19]=3)=[O:15])[C@H:11]([C:27](=[O:37])[NH:28][CH:29]([CH3:36])[CH2:30][N:31]3[CH2:35][CH2:34][CH2:33][CH2:32]3)[CH2:10]2)=CC=1.FC(F)(F)C(O)=O.[F:47][C:48]([F:54])([F:53])[S:49]([OH:52])(=[O:51])=[O:50]>C1(OC)C=CC=CC=1>[F:47][C:48]([F:54])([F:53])[S:49]([OH:52])(=[O:51])=[O:50].[F:47][C:48]([F:54])([F:53])[S:49]([OH:52])(=[O:51])=[O:50].[SH:8][C@@H:9]1[CH2:13][N:12]([C:14]([O:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][CH:19]=2)=[O:15])[C@H:11]([C:27](=[O:37])[NH:28][CH:29]([CH3:36])[CH2:30][N:31]2[CH2:35][CH2:34][CH2:33][CH2:32]2)[CH2:10]1

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 62406Trifluoromethanesulfonic acidHCID 67781019(2S, 4S)-4-(4-methoxybenzylthio)-2-(1-methyl-2-pyrrolidinylethylcarbamoyl)-1-(4-nitrobenzyloxycarbonyl)pyrrolidine

生成物 1

HCID 86747836(2S, 4S)-4-Mercapto-2-(1-methyl-2-pyrrolidinylethylcarbamoyl)-1-(4-nitrobenzyloxycarbonyl)pyrrolidine bis(trifluoromethanesulfonate)

試薬・触媒・溶媒 1

HCID 7519Anisole溶媒

実験手順

369 mg of (2S, 4S)-4-(4-methoxybenzylthio)-2-(1-methyl-2-pyrrolidinylethylcarbamoyl)-1-(4-nitrobenzyloxycarbonyl)pyrrolidine (prepared as described in Preparation 2) were suspended in 720 μl of anisole, and the suspension was placed on an ice bath. Maintaining the suspension on the ice bath, 3.6 ml of trifluoroacetic acid and 128 μl of trifluoromethanesulfonic acid were added to it, and it was then stirred for 1 hour at room temperature. At the end of this time, the solvent was removed by distillation under reduced pressure. The residue was washed with diethyl ether by repeated decantation and dried under reduced pressure, to give 440 mg of the title compound.

後処理

  1. customthe suspension was placed on an ice bath
  2. additionwere added to it, and it
  3. customAt the end of this time, the solvent was removed by distillation under reduced pressure
  4. washThe residue was washed with diethyl ether by repeated decantation
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-9936235296c34f62be8d9c89d6719f17
出典データセット
uspto-grants-1994_05
特許番号
US05310735

関連ノート

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