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Ammonium Chloride → HCID 86664655, 화합물

HRID 1917404
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HRID 1917404 반응식
[CH2:1]1CCN2C(=NCCC2)CC1.C[N+](C)=C.[I-].[C:17]([O:21][C:22]([C@@:24]1([CH2:38][CH2:39][CH:40]=[O:41])[CH2:28][C:27](=[O:29])[N:26]([C@@H:30]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH3:31])[CH2:25]1)=[O:23])([CH3:20])([CH3:19])[CH3:18].[Cl-].[NH4+]>ClCCl>[C:17]([O:21][C:22]([C@@:24]1([CH2:38][C:39](=[CH2:1])[CH:40]=[O:41])[CH2:28][C:27](=[O:29])[N:26]([C@@H:30]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH3:31])[CH2:25]1)=[O:23])([CH3:20])([CH3:19])[CH3:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 25517Ammonium ChlorideHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 2724133Dimethyl(methylene)ammounium iodide2회HCID 86664654(3S)-3-(3-Oxo-1-propyl)-5-oxo-1-[(1R)-1-phenylethyl]pyrrolidine-3-carboxylic acid tert-butyl ester

생성물 1

HCID 86664655HCID 86664655, 화합물

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

1,8-Diazabicyclo[5.4.0]-7-undecene (2.17 ml, 14.5 mmol) and Eschenmoser salt (3.66 g, 19.8 mmol) were added to a solution of (3S)-3-(3-oxo-1-propyl)-5-oxo-1-[(1R)-1-phenylethyl]pyrrolidine-3-carboxylic acid tert-butyl ester in dichloromethane (88.0 ml) in a nitrogen atmosphere, and the mixture was stirred at room temperature for 16 hours. Thereafter, Eschenmoser salt (1.22 g, 6.59 mmol) was added, and the mixture was stirred at room temperature for three hours. A saturated ammonium chloride solution (150 ml) was added to the reaction solution, followed by extraction with chloroform (100 ml×1, 150 ml×1). The organic layer was washed with brine (200 ml) and then dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0→90:10→66:34→60:40→50:50→34:66) to give 3.14 g of the title compound as white crystals.

후처리

  1. stirringthe mixture was stirred at room temperature for three hours
  2. extractionfollowed by extraction with chloroform (100 ml×1, 150 ml×1)
  3. washThe organic layer was washed with brine (200 ml)
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationAfter filtration
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0→90:10→66:34→60:40→50:50→34:66)

출처 및 근거

ORD 기록
ord-f7aa2a94ed394d919730325a1a8514cc
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08618094B2

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