Ethyl alpha-benzylacetoacetate → HCID 136026728, Verbindung

HRID 1718249Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1718249
F[B-](F)(F)F.[C:6](=[NH:11])([O:8][CH2:9][CH3:10])[NH2:7].[CH2:12]([CH:19]([C:25](=O)[CH3:26])[C:20](OCC)=[O:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C[O-].[Na+]>CO>[CH2:12]([C:19]1[C:20](=[O:21])[NH:11][C:6]([O:8][CH2:9][CH3:10])=[N:7][C:25]=1[CH3:26])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

Komponenten

5

Edukt 3

HCID 246929Ethyl alpha-benzylacetoacetateHCID 10942334Sodium MethoxideHCID 86622837Ethyl imidocarbamate tetrafluoroborate

Produkt 1

HCID 136026728HCID 136026728, VerbindungAusbeute 24,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of ethyl imidocarbamate tetrafluoroborate (2.4 g) and ethyl 2-benzyl-3-oxobutanoate (1 g) in methanol (20 mL) was added sodium methoxide (28% methanol solution, 5.25 mL), and the mixture was stirred for 12 hr. The reaction mixture was concentrated, and the residue was dissolved in water. The solution was weakly acidified with acetic acid, extracted with ethyl acetate, washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was crystallized from diisopropyl ether to give the title compound (0.27 g, 24%) as a colorless solid.

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in water
  3. extractionextracted with ethyl acetate
  4. washwashed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customThe residue was crystallized from diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-88d7a01c6b524e1f9cef05f5a142b496
Quelldatensatz
uspto-grants-2010_09
Patentnummer
US07803940B2

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