Hydrochloric Acid → (2S,4S)-4-(4-Methoxybenzylthio)-2-(1-piperazinyl-carbonyl)-1-(4-nitrobenzyloxycarbonyl)pyrrolidine hydrochloride

HRID 727620ノート

反応式

HRID 727620 の反応式
[ClH:1].[CH3:2][O:3][C:4]1[CH:44]=[CH:43][C:7]([CH2:8][S:9][C@@H:10]2[CH2:14][N:13]([C:15]([O:17][CH2:18][C:19]3[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=3)=[O:16])[C@H:12]([C:28]([N:30]3[CH2:35][CH2:34][N:33](C(OC(C)(C)C)=O)[CH2:32][CH2:31]3)=[O:29])[CH2:11]2)=[CH:6][CH:5]=1>C(OCC)(=O)C>[ClH:1].[CH3:2][O:3][C:4]1[CH:5]=[CH:6][C:7]([CH2:8][S:9][C@@H:10]2[CH2:14][N:13]([C:15]([O:17][CH2:18][C:19]3[CH:20]=[CH:21][C:22]([N+:25]([O-:27])=[O:26])=[CH:23][CH:24]=3)=[O:16])[C@H:12]([C:28]([N:30]3[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]3)=[O:29])[CH2:11]2)=[CH:43][CH:44]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 57015053(2S,4S)-4-(4-Methoxybenzylthio)-2-(4-t-butoxycarbonylpiperazin-1-ylcarbonyl)-1-(4-nitrobenzyloxycarbonyl)pyrrolidine

生成物 1

HCID 67585358(2S,4S)-4-(4-Methoxybenzylthio)-2-(1-piperazinyl-carbonyl)-1-(4-nitrobenzyloxycarbonyl)pyrrolidine hydrochloride

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

27 ml of a 4N ethyl acetate solution of hydrogen chloride were added to a solution of 5.2 g of (2S,4S)-4-(4-methoxybenzylthio)-2-(4-t-butoxycarbonylpiperazin-1-ylcarbonyl)-1-(4-nitrobenzyloxycarbonyl)pyrrolidine [prepared as described in step (i) above] in 27 ml of ethyl acetate, and the resulting mixture was heated under reflux for 2 hours. At the end of this time, the reaction mixture was concentrated to dryness by evaporation under reduced pressure, and the resulting concentrate was triturated with diethyl ether. The powder thus obtained was collected by filtration and dried to give 4.2 g of the title compound.

後処理

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 2 hours
  3. concentrationAt the end of this time, the reaction mixture was concentrated to dryness by evaporation under reduced pressure
  4. concentrationthe resulting concentrate
  5. customwas triturated with diethyl ether
  6. customThe powder thus obtained
  7. filtrationwas collected by filtration
  8. customdried

出典と根拠

ORDレコード
ord-9bd60dc1c00a4478ab5d8d8efa3517db
出典データセット
uspto-grants-1998_01
特許番号
US05712267

反応ノート

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