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Diisopropylamine → Dibenzyl 2-isopropyl-2-hydroxy-3-methylsuccinate

HRID 1774383
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1774383
C(NC(C)C)(C)C.O1CCCC1.C([N-]C(C)C)(C)C.[Li+].[C:21]([O:25][CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)(=[O:24])[CH2:22][CH3:23].[CH3:33][CH:34]([CH3:47])[C:35](=[O:46])[C:36]([O:38][CH2:39][C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1)=[O:37]>O1CCCC1.C(O)(=O)CC(CC(O)=O)(C(O)=O)O.CCCCCC.C(OCC)(=O)C>[CH:34]([C:35]([OH:46])([CH:22]([CH3:23])[C:21]([O:25][CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)=[O:24])[C:36]([O:38][CH2:39][C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1)=[O:37])([CH3:47])[CH3:33]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 7912DiisopropylamineHCID 31219Benzyl propionateHCID 10997623Lithium diisopropylamide mono(tetrahydrofuran)HCID 11160044Benzyl 3-methyl-2-oxobutanoate

Produkt 1

HCID 66648722Dibenzyl 2-isopropyl-2-hydroxy-3-methylsuccinateAusbeute 66 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 311
Citric Acid
Lösungsmittel
HCID 8028TetrahydrofuranLösungsmittel3×
HCID 21226206Ethyl acetate hexaneLösungsmittel

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

To anhydrous tetrahydrofuran (5 mL) was added diisopropylamine (759 mg, 7.5 mmol) under nitrogen stream, and the mixture was cooled to −78° C. To the solution was added a 1.58 M n-butyl lithium-hexane solution (4.3 mL, 6.8 mmol), and the mixture was stirred at −78° C. for 5 min, and then at 0° C. for 15 min. The solution of lithium diisopropylamide tetrahydrofuran was cooled to −78° C., and a solution of benzyl propionate (821 mg, 5.0 mmol) in anhydrous tetrahydrofuran (10 mL) was added dropwise over 1 h, and the reaction mixture was further stirred at −78° C. for 1 h. The enolate thus prepared was added via a cannula to a solution of benzyl 3-methyl-2-ketobutyrate (1.24 g, 6.0 mmol) in anhydrous tetrahydrofuran (5 mL) having been cooled to −78° C. After stirring at −78° C. for 2 h, the reaction mixture was diluted with a 10% aqueous citric acid solution, and extracted with ethyl acetate. The organic layer was washed with 1 M hydrochloric acid, saturated aqueous sodium hydrogen carbonate and brine, dried over anhydrous magnesium sulfate, and filtered. The solvent was evaporated under reduced pressure, and the residue thus obtained was subjected to silica gel column chromatography (hexane-ethyl acetate 9:1) to give 1.22 g of dibenzyl 2-isopropyl-2-hydroxy-3-methylsuccinate as oil (yield: 66%) in the form of a diastereomer mixture.

Aufarbeitung

  1. additionTo the solution was added a 1.58 M n-butyl lithium-hexane solution (4.3 mL, 6.8 mmol)
  2. waitat 0° C. for 15 min
  3. stirringthe reaction mixture was further stirred at −78° C. for 1 h
  4. temperaturehaving been cooled to −78° C
  5. stirringAfter stirring at −78° C. for 2 h
  6. extractionextracted with ethyl acetate
  7. washThe organic layer was washed with 1 M hydrochloric acid, saturated aqueous sodium hydrogen carbonate and brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. filtrationfiltered
  10. customThe solvent was evaporated under reduced pressure
  11. customthe residue thus obtained

Quellen und Nachweise

ORD-Eintrag
ord-c3bfdbfb56dc4b4691b441743fe77d2b
Quelldatensatz
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09260375B2

Notizen zur Reaktion

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