3-Methyl-2-butanone → HCID 59487984, Verbindung

HRID 1881392Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1881392
C(OC(=O)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11](=[O:18])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)C.C[C:21](C)([O-:23])C.[K+].[CH3:26][CH:27]([CH3:31])[C:28](=[O:30])[CH3:29]>C1COCC1>[C:11]([C:6]1[CH:5]=[CH:10][C:9]([C:21](=[O:23])[CH2:29][C:28](=[O:30])[CH:27]([CH3:31])[CH3:26])=[CH:8][CH:7]=1)(=[O:18])[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

Komponenten

5

Edukt 3

HCID 112513-Methyl-2-butanoneHCID 221768Ethyl o-benzoylbenzoateHCID 23665647Potassium tert-butoxide

Produkt 1

HCID 59487984HCID 59487984, VerbindungAusbeute 87,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

10 g (39 mmol) of benzoylbenzoic ethylester are added to a suspension of 3.94 g (35 mmol) of potassium-tert-butoxid in 60 ml of THF at 0° C. under argon. 2.82 g (33 mmol) of 3-methyl-2-butanone are added in 1 h while the temperature rises to 25° C. After 2 h at 40° C. the reaction mixture is poured into 500 ml of ice water containing 10 ml conc. HCl. Extraction with toluene and evaporation gives the crude product (8.5 g) which is purified by crystallisation in heptane yielding 3.7 g of a white solid. The structure is confirmed by 1H-NMR and 13C-NMR spectra. mp: 76.5-78° C.

Aufarbeitung

  1. customrises to 25° C
  2. extractionExtraction
  3. customwith toluene and evaporation

Quellen und Nachweise

ORD-Eintrag
ord-68b8389eaf4b4f6dbfe03b8110b546cd
Quelldatensatz
uspto-grants-2012_11
Patentnummer
US08318830B2

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