Ammonium Chloride → 4-Methyl-4-phenyl-3,4-dihydro-1H-quinazolin-2-one

HRID 1497734

Reaktionsgleichung

Reaktionsgleichung von HRID 1497734
[C:1]1([C:7]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[NH:10][C:9](=[O:17])[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:18][Mg]Br.[NH4+].[Cl-]>C1COCC1>[CH3:18][C:7]1([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[NH:10][C:9](=[O:17])[NH:8]1

Komponenten

5

Edukt 3

HCID 25517Ammonium ChlorideHCID 634302(1H)-Quinazolinone, 4-phenyl-HCID 178418573HCID 178418573, Verbindung

Produkt 1

HCID 1176010134-Methyl-4-phenyl-3,4-dihydro-1H-quinazolin-2-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 4-Phenyl-1H-quinazolin-2-one (5.0 g, 4.5 mmol) in THF (50 ml) is added methylmagnesium bromide (15.0 ml) dropwise at −78° C. under nitrogen. The mixture is stirred overnight at room temperature. The mixture is poured into an aqueous solution of NH4Cl and then extracted with EtOAc. The organic phase is washed with brine, dried over Na2SO4, filtered and evaporated under reduced pressure. The residue is purified on silica gel to give product as a white solid.

Aufarbeitung

  1. extractionextracted with EtOAc
  2. washThe organic phase is washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. customThe residue is purified on silica gel
  7. customto give product as a white solid

Quellen und Nachweise

ORD-Eintrag
ord-2394edaa774548dda0671e282f6907e3
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09199988B2

Verknüpfte Notizen

Wird geladen…