Reaktionsgleichung
[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:20][CH3:21])=[C:6]([C:8]([CH3:19])([CH3:18])[CH2:9][C:10](N2CCOCC2)=[O:11])[CH:7]=1.[CH3:22][Li]>C1COCC1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:20][CH3:21])=[C:6]([C:8]([CH3:18])([CH3:19])[CH2:9][C:10](=[O:11])[CH3:22])[CH:7]=1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a solution of 3-(5-fluoro-2-methoxyphenyl)-3-methyl-1-morpholin-4-ylbutan-1-one (0.59 g) in THF (1 mL) stirred under argon and cooled on dry ice/acetone was added methyl lithium (1.4 M in pentane, 2 mL) over 2 minutes. The mixture was stirred for 30 minutes and quenched with EtOH (0.3 mL). The mixture was warmed to room temperature and 1 mL of water was added. The organic phase was separated, washed, dried, filtered, and evaporated. The residue was fractionated over a short column of silica gel (eluent: hexanes-methylene chloride (1:1)) to give the title compound as an oil (0.36 g).
Aufarbeitung
- temperaturecooled on dry ice/acetone
- customquenched with EtOH (0.3 mL)
- addition1 mL of water was added
- customThe organic phase was separated
- washwashed
- customdried
- filtrationfiltered
- customevaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-3da18985e3cf40d98df5062c234e3bcd
- Quelldatensatz
- uspto-grants-2005_06
- Patentnummer
- US06903215B2
Verknüpfte Notizen
Wird geladen…