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Triethylamine → 4-(S)-benzyl-3-(3-(R)-hydroxy-2-(S)-methyl-7-phenylheptanoyl)oxazolidin-2-one

HRID 1107149
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1107149
[CH2:1]([C@H:8]1[CH2:12][O:11][C:10](=[O:13])[N:9]1[C:14](=[O:17])[CH2:15][CH3:16])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[O-]S(C(F)(F)F)(=O)=O.C([B+]CCCC)CCC.C(N(CC)CC)C.C(=O)=O.CC(C)=O.[C:49]1([CH2:55][CH2:56][CH2:57][CH2:58][CH:59]=[O:60])[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=1>C(Cl)Cl>[CH2:1]([C@H:8]1[CH2:12][O:11][C:10](=[O:13])[N:9]1[C:14](=[O:17])[C@@H:15]([CH3:16])[C@H:59]([OH:60])[CH2:58][CH2:57][CH2:56][CH2:55][C:49]1[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 8471TriethylamineHCID 561886BenzenepentanalHCID 2733696(4S)-4-Benzyl-3-propanoyl-1,3-oxazolidin-2-oneHCID 18522661Acetone cardiceHCID 178418657HCID 178418657, Verbindung

Produkt 1

HCID 21968326
4-(S)-benzyl-3-(3-(R)-hydroxy-2-(S)-methyl-7-phenylheptanoyl)oxazolidin-2-one
Ausbeute 70 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel3×

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

4-(S)-Benzyl-3-propionyl-2-oxazolidinone (8.4 g, 36 mmol) is dissolved in CH2Cl2 (60 mL), cooled in an ice bath and to this is added 1 M dibutyl boron triflate in CH2Cl2 (40 mL, 40 mmol) over 5 minutes. Then triethylamine (6.3 mL, 45 mmol) is added dropwise at a rate that kept the reaction temperature <3° C. The ice bath is then replaced by dry-ice/acetone and 5-phenylpentanal (7.8 g, 48 mmol) in CH2Cl2 (20 mL) is added over 5 minutes. This mixture is stirred 20 minutes at -78° C. and then for 1 hour at 0° C. The reaction is quenched by the addition of pH 7 phosphate buffer (40 mL), followed by MeOH (120 mL). Then a mixture of MeOH (80 mL) and 30% hydrogen peroxide (40 mL) is added at a rate that kept the reaction temperature <10° C. The reaction is stirred 1 hour and then concentrated in vacuo (bath temperature <30° C.). The residue is extracted into ether (3×200 mL) and the combined ether layers are washed with NaHCO3 (200 mL), brine (200 mL) and dried over MgSO4 and then concentrated in vacuo. The crude product is purified by column chromatography (silica, 10% petroleum ether in CH2Cl2 then a second purification using 45% ether in petroleum ether) to yield 4-(S)-benzyl-3-(3-(R)-hydroxy-2-(S)-methyl-7-phenylheptanoyl)oxazolidin-2-one (9.8 g, 70%): 1H NMR (300 MHz, CDCl3) δ 7.37-7.14 (m, 10H), 4.73-4.65 (m,1H), 4.24-4.15 (m, 2H), 3.96-3.91 (m, 1H), 3.79-3.71 (m, 1H), 3.27-3.21 (dd, J=13.4, 3.3 Hz, 1H), 2.88 (d, J=3.0 Hz, 1H), 2.78 (dd, J=13.3, 9.5 Hz, 1H), 2.62 (t, J=7.5 Hz, 2H), 1.70-1.34 (m, 6H), 1.25 (d, J=6.8 Hz, 3H).

Aufarbeitung

  1. temperaturecooled in an ice bath
  2. customthe reaction temperature <3° C
  3. additionis added over 5 minutes
  4. waitfor 1 hour at 0° C
  5. customThe reaction is quenched by the addition of pH 7 phosphate buffer (40 mL)
  6. additionThen a mixture of MeOH (80 mL) and 30% hydrogen peroxide (40 mL)
  7. additionis added at a rate that
  8. customthe reaction temperature <10° C
  9. stirringThe reaction is stirred 1 hour
  10. concentrationconcentrated in vacuo (bath temperature <30° C.)
  11. extractionThe residue is extracted into ether (3×200 mL)
  12. washthe combined ether layers are washed with NaHCO3 (200 mL), brine (200 mL)
  13. dry with materialdried over MgSO4
  14. concentrationconcentrated in vacuo
  15. customThe crude product is purified by column chromatography (silica, 10% petroleum ether in CH2Cl2
  16. customa second purification

Quellen und Nachweise

ORD-Eintrag
ord-9dc304c20b3a4ad7b5b49b733c00c982
Quelldatensatz
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06057369

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