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N-bromobutanimide → (4R)-4-benzyl-3-[(2R)-2-bromo-3-butylheptanoyl]-1,3-oxazolidin-2-one

HRID 1815633
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1815633
[CH2:1]([Mg]Cl)[CH2:2][CH2:3][CH3:4].[CH2:7]([C@@H:14]1[CH2:18][O:17][C:16](=[O:19])[N:15]1[C:20](=[O:27])/[CH:21]=[CH:22]/[CH2:23][CH2:24][CH2:25][CH3:26])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[Br:28]N1C(=O)CCC1=O>C1COCC1.CSC>[CH2:7]([C@@H:14]1[CH2:18][O:17][C:16](=[O:19])[N:15]1[C:20](=[O:27])[C@H:21]([Br:28])[CH:22]([CH2:1][CH2:2][CH2:3][CH3:4])[CH2:23][CH2:24][CH2:25][CH3:26])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 67184N-bromobutanimideHCID 66929717(4R)-4-benzyl-3-[(E)-2-heptenoyl]-1,3-oxazolidin-2-oneHCID 178418265HCID 178418265, Verbindung

Produkt 1

HCID 66929892(4R)-4-benzyl-3-[(2R)-2-bromo-3-butylheptanoyl]-1,3-oxazolidin-2-one

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1068Dimethyl SulfideLösungsmittel
HCID 8028
Tetrahydrofuran
Lösungsmittel
2×

Reaktionsbedingungen

Temperatur
-15 °C

Versuchsvorschrift

A slurry of copper bromide(I) dimethyl sulfide complex (5.132 g, 24.967 mmol) in THF (60 mL) and dimethyl sulfide (30 mL) as a co-solvent was cooled to −40° C. and n-butyl magnesium chloride (25 mL, 49.93 mmol) was added dropwise for 10 min and stirred for 20 min while warming to −15° C. The black slurry was cooled to −40° C. and (4R)-4-benzyl-3-[(E)-2-heptenoyl]-1,3-oxazolidin-2-one (6 g, 20.80 mmol) was added dropwise over 10 min as a solution in THF (20 mL) at −40° C. The reaction was let warm up to 25° C. overnight (20 h). N-Bromosuccinimide (7.407 g, 41.61 mmol) was added portionwise to a cold −78° C. solution of the black slurry. It was allowed to warm to 0° C. and was stirred for an additional 3 h. The reaction was quenched with a 1:1 solution of saturated ammonium carbonate and 0.5 N potassium bisulfate. The black slurry became greenish to blue. A precipitate formed (light blue). It was filtered. The mother liquor was diluted with ethyl acetate (150 mL) and the organic was dried over MgSO4, filtered, concentrated to obtain (4R)-4-benzyl-3-[(2R)-2-bromo-3-butylheptanoyl]-1,3-oxazolidin-2-one as a crude semi-solid (green) (8.49 g, 96.15%). Mass Spectrum (−ESI): 423 (M−H)−.

Aufarbeitung

  1. temperatureThe black slurry was cooled to −40° C.
  2. temperatureThe reaction was let warm up to 25° C. overnight (20 h)
  3. temperatureto warm to 0° C.
  4. stirringwas stirred for an additional 3 h
  5. customThe reaction was quenched with a 1:1 solution of saturated ammonium carbonate and 0.5 N potassium bisulfate
  6. customA precipitate formed (light blue)
  7. filtrationIt was filtered
  8. additionThe mother liquor was diluted with ethyl acetate (150 mL)
  9. dry with materialthe organic was dried over MgSO4
  10. filtrationfiltered
  11. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-c1f4bb7b4b124d8887a7dc58bffdc48f
Quelldatensatz
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06878742B2

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