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

HRID 727620노트

반응식

HRID 727620 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9bd60dc1c00a4478ab5d8d8efa3517db
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05712267

반응 노트

불러오는 중…