HCID 22398528, Verbindung → 4-(5-Fluoro-2-methoxyphenyl)-4-methylpentan-2-one

HRID 916022Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 916022
[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]=1

Komponenten

4

Edukt 2

HCID 22398528HCID 22398528, VerbindungHCID 178418348HCID 178418348, Verbindung

Produkt 1

HCID 222849224-(5-Fluoro-2-methoxyphenyl)-4-methylpentan-2-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of the above 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 4-(5-fluoro-2-methoxyphenyl)-4-methylpentan-2-one as an oil (0.36 g).

Aufarbeitung

  1. temperaturecooled on dry ice/acetone
  2. customquenched with EtOH (0.3 mL)
  3. addition1 mL of water was added
  4. customThe organic phase was separated
  5. washwashed
  6. customdried
  7. filtrationfiltered
  8. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-d156692828644d96932c461e2b2ae425
Quelldatensatz
uspto-grants-2007_09
Patentnummer
US07268152B2

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