Acetone → 1-(2,4-Difluorophenyl)-2-methylpropan-2-ol

HRID 12103Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 12103
[CH3:1][C:2]([CH3:4])=[O:3].[F:5][C:6]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:7]=1[CH2:8][Mg]Br.[Cl-].[NH4+]>C(OCC)C>[F:5][C:6]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:7]=1[CH2:8][C:2]([CH3:4])([OH:3])[CH3:1]

Komponenten

5

Edukt 3

HCID 180AcetoneHCID 25517Ammonium ChlorideHCID 178505754HCID 178505754, Verbindung

Produkt 1

HCID 220634481-(2,4-Difluorophenyl)-2-methylpropan-2-ol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

11.0 mL acetone, diluted with 50 mL diethyl ether, is added dropwise to a solution of 500 mL of 0.25 molar 2,4-difluorobenzylmagnesium bromide in diethyl ether within 20 minutes. Then the mixture is refluxed for 1.5 hours and then hydrolyzed with 10% ammonium chloride solution. The ether phase is separated off, washed with water, dried with sodium sulfate, and evaporated down. The fractional distillation of the residue yields the alcohol as a colorless liquid (boiling point: 70° C.-73° C./2 mmbar). Yield: 20.0 g (86%).

Aufarbeitung

  1. temperatureThen the mixture is refluxed for 1.5 hours
  2. customThe ether phase is separated off
  3. washwashed with water
  4. dry with materialdried with sodium sulfate
  5. customevaporated down
  6. distillationThe fractional distillation of the residue

Quellen und Nachweise

ORD-Eintrag
ord-09a95e78dab74866bdc4b0f4e523c6ac
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07727984B2

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