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Thiophenol → {(S)-2-[4-(2-Chlorophenyl)-2,2-dimethyl-5-oxopiperazin-1-yl]-1-[(2S,4R)-5-oxo-4-propyltetrahydrofuran-2-yl]ethyl}carbamic acid t-butyl ester

HRID 1695014
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HRID 1695014 반응식
[C:1](=[O:4])([O-:3])[O-].[Cs+].[Cs+].[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[N:14]1[C:19](=[O:20])[CH2:18][N:17]([CH2:21][C@H:22]([NH:32]S(C2C=CC=CC=2[N+]([O-])=O)(=O)=O)[C@@H:23]2[CH2:27][C@@H:26]([CH2:28][CH2:29][CH3:30])C(=O)O2)[C:16]([CH3:46])([CH3:45])[CH2:15]1.C1(S)C=CC=CC=1.C(=O)(O)[O-].[Na+].[C:59](OC(OC(C)(C)C)=O)([O:61][C:62]([CH3:65])([CH3:64])[CH3:63])=[O:60].N[C@H]([C@@H]1C[C@@H](CCC)C(=O)O1)CN1C(C)(C)CN(C2C=CC=CC=2Cl)C(=O)C1>C(#N)C.[Cl-].[Na+].O.C(OCC)(=O)C.O>[C:62]([O:61][C:59](=[O:60])[NH:32][C@H:22]([C@@H:23]1[CH2:27][C@@H:26]([CH2:28][CH2:29][CH3:30])[C:1](=[O:4])[O:3]1)[CH2:21][N:17]1[CH2:18][C:19](=[O:20])[N:14]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[Cl:7])[CH2:15][C:16]1([CH3:45])[CH3:46])([CH3:65])([CH3:64])[CH3:63]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 6

HCID 7969ThiophenolHCID 10796Cesium carbonateHCID 90495Di-tert-butyl dicarbonateHCID 516892Sodium BicarbonateHCID 666457934-{(S)-2-amino-2-[(2S,4R)-5-oxo-4-propyltetrahydrofuran-2-yl]ethyl}-1-(2-chlorophenyl)-5,5-dimethylpiperazin-2-one
HCID 66645872
N-{(S)-2-[4-(2-Chlorophenyl)-2,2-dimethyl-5-oxopiperazin-1-yl]-1-[(2S,4R)-5-oxo-4-propyltetrahydrofuran-2-yl]ethyl}-2-nitrobenzenesulfonamide

생성물 1

HCID 66645802{(S)-2-[4-(2-Chlorophenyl)-2,2-dimethyl-5-oxopiperazin-1-yl]-1-[(2S,4R)-5-oxo-4-propyltetrahydrofuran-2-yl]ethyl}carbamic acid t-butyl ester수율 73.5%

시약·촉매·용매 4

HCID 962Water용매HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매HCID 57417360Sodium chloride; water용매2회

실험 절차

585 mg of cesium carbonate (1.8 mmol) was added to a solution of 888 mg of N-{(S)-2-[4-(2-chlorophenyl)-2,2-dimethyl-5-oxopiperazin-1-yl]-1-[(2S,4R)-5-oxo-4-propyltetrahydrofuran-2-yl]ethyl}-2-nitrobenzenesulfonamide obtained in Example (116h) (1.50 mmol) and 0.46 ml of thiophenol (content: 95%) (4.5 mmol) in acetonitrile (15 ml) under a nitrogen atmosphere at room temperature, and the mixture was stirred at the same temperature for 2.5 hours. Brine was added to the reaction mixture, followed by extraction with methylene chloride. Then, the organic layer was dried over anhydrous magnesium sulfate. After filtration, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (elution solvent:methylene chloride/methanol=50/1-10/1). 94 mg of sodium bicarbonate (1.12 mmol) and 245 mg of di-t-butyl dicarbonate (1.12 mmol) were added to a solution of 4-{(S)-2-amino-2-[(2S,4R)-5-oxo-4-propyltetrahydrofuran-2-yl]ethyl}-1-(2-chlorophenyl)-5,5-dimethylpiperazin-2-one obtained above in ethyl acetate (5 ml)-water (5 ml), and the mixture was stirred at room temperature overnight. Brine was added to the reaction mixture, followed by extraction with ethyl acetate. Then, the organic layer was dried over anhydrous magnesium sulfate. After filtration, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (elution solvent:methylene chloride/methanol=40/1-20/1) to obtain 418 mg of the title compound (yield: 55%).

후처리

  1. extractionfollowed by extraction with methylene chloride
  2. dry with materialThen, the organic layer was dried over anhydrous magnesium sulfate
  3. filtrationAfter filtration
  4. customthe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (elution solvent:methylene chloride/methanol=50/1-10/1)
  6. stirringthe mixture was stirred at room temperature overnight
  7. extractionfollowed by extraction with ethyl acetate
  8. dry with materialThen, the organic layer was dried over anhydrous magnesium sulfate
  9. filtrationAfter filtration
  10. customthe solvent was evaporated under reduced pressure
  11. customthe residue was purified by silica gel column chromatography (elution solvent:methylene chloride/methanol=40/1-20/1)

출처 및 근거

ORD 기록
ord-953142a355114b759bdae603202ccfa9
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08158790B2

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