Trifluoroacetic acid → (2S,4S)-4-Mercapto-2-[4-(2-hydroxyethyl)-1-piperazinylcarbonyl)-1-methylpyrrolidine bis(trifluoromethanesulfonate)

HRID 362065ノート

反応式

HRID 362065 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].[OH:16][CH2:17][CH2:18][N:19]1[CH2:24][CH2:23][N:22]([C:25]([C@@H:27]2[CH2:31][C@H:30]([S:32]CC3C=CC(OC)=CC=3)[CH2:29][N:28]2[CH3:42])=[O:26])[CH2:21][CH2:20]1>C1(OC)C=CC=CC=1>[F:8][C:9]([F:15])([F:14])[S:10]([OH:13])(=[O:12])=[O:11].[F:8][C:9]([F:15])([F:14])[S:10]([OH:13])(=[O:12])=[O:11].[SH:32][C@@H:30]1[CH2:29][N:28]([CH3:42])[C@H:27]([C:25]([N:22]2[CH2:21][CH2:20][N:19]([CH2:18][CH2:17][OH:16])[CH2:24][CH2:23]2)=[O:26])[CH2:31]1

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 62406Trifluoromethanesulfonic acidHCID 67612520HCID 67612520、化合物

生成物 1

HCID 86753695(2S,4S)-4-Mercapto-2-[4-(2-hydroxyethyl)-1-piperazinylcarbonyl)-1-methylpyrrolidine bis(trifluoromethanesulfonate)

試薬・触媒・溶媒 1

HCID 7519Anisole溶媒

実験手順

10 ml of trifluoroacetic acid and 520 μl of trifluoromethanesulfonic acid were added, whilst ice-cooling, to a solution of 1150 mg of (2S,4S)-2-[4-(2-hydroxyethyl)-1-piperazinylcarbonyl)-4-(4-methoxybenzylthio)-1-methylpyrrolidine [prepared as described in step (i) above] in 3 ml of anisole, and the resulting mixture was stirred at room temperature for 1 hour. At the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure, to give 1680 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

出典と根拠

ORDレコード
ord-981708e218db43f6bd29d99133da710c
出典データセット
uspto-grants-1999_02
特許番号
US05866564

反応ノート

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