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Ammonium Chloride → (3S)-3-(3-Hydroxy-2-methylene-1-propyl)-5-oxo-1-[(1R)-1-phenylethyl]pyrrolidine-3-carboxylic acid tert-butyl ester

HRID 1917405
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1917405
[BH4-].[Na+].O.O.O.O.O.O.O.[Cl-].[Ce+3].[Cl-].[Cl-].[C:14]([O:18][C:19]([C@@:21]1([CH2:35][C:36](=[CH2:39])[CH:37]=[O:38])[CH2:25][C:24](=[O:26])[N:23]([C@@H:27]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH3:28])[CH2:22]1)=[O:20])([CH3:17])([CH3:16])[CH3:15].[Cl-].[NH4+]>C(O)C>[C:14]([O:18][C:19]([C@@:21]1([CH2:35][C:36](=[CH2:39])[CH2:37][OH:38])[CH2:25][C:24](=[O:26])[N:23]([C@@H:27]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH3:28])[CH2:22]1)=[O:20])([CH3:16])([CH3:15])[CH3:17]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 25517Ammonium ChlorideHCID 4311764Sodium borohydride2×HCID 21585214Cerium trichloride heptahydrate2×HCID 86664655HCID 86664655, Verbindung

Produkt 1

HCID 67490972(3S)-3-(3-Hydroxy-2-methylene-1-propyl)-5-oxo-1-[(1R)-1-phenylethyl]pyrrolidine-3-carboxylic acid tert-butyl ester
Ausbeute 120,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Ethanol (43.9 ml) was added to sodium borohydride (644 mg, 17.0 mmol) in a nitrogen atmosphere, and the mixture was cooled with ice-acetone. Cerium chloride heptahydrate (6.55 g, 17.6 mmol) and (3S)-3-(3-oxo-2-methylene-1-propyl)-5-oxo-1-[(1R)-1-phenylethyl]pyrrolidine-3-carboxylic acid tert-butyl ester (3.14 g, 6.55 mmol) were added under cooling. The mixture was stirred under cooling for one hour, and then cerium chloride heptahydrate (1.64 g, 4.40 mmol) and sodium borohydride (166 mg, 4.39 mmol) were added. The mixture was stirred under cooling for 30 minutes and then ice-cooled. A saturated ammonium chloride solution (150 ml) was added to the reaction solution. The mixture was concentrated under reduced pressure and ethanol was removed. The mixture was extracted with ethyl acetate (150 ml×1, 100 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→50:50→34:66→25:75→17:83→5:95) to give 2.83 g of the title compound.

Aufarbeitung

  1. temperatureunder cooling
  2. temperatureunder cooling for one hour
  3. stirringThe mixture was stirred
  4. temperatureunder cooling for 30 minutes
  5. temperatureice-cooled
  6. concentrationThe mixture was concentrated under reduced pressure and ethanol
  7. customwas removed
  8. extractionThe mixture was extracted with ethyl acetate (150 ml×1, 100 ml×1)
  9. washThe organic layer was washed with brine (200 ml)
  10. dry with materialdried over anhydrous sodium sulfate
  11. filtrationAfter filtration
  12. concentrationthe filtrate was concentrated under reduced pressure
  13. customThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0→90:10→66:34→50:50→34:66→25:75→17:83→5:95)

Quellen und Nachweise

ORD-Eintrag
ord-e7036df58f2e4821814b560cb28118a9
Quelldatensatz
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08618094B2

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