Potassium Carbonate → (4-(2,6-Difluorobenzyloxy)phenyl)-acetonitrile

HRID 25017

Reaktionsgleichung

Reaktionsgleichung von HRID 25017
[OH:1][C:2]1[CH:10]=[CH:9][C:5]([CH2:6][C:7]#[N:8])=[CH:4][CH:3]=1.C([O-])([O-])=O.[K+].[K+].[F:17][C:18]1[CH:25]=[CH:24][CH:23]=[C:22]([F:26])[C:19]=1[CH2:20]Br>CN(C=O)C>[F:17][C:18]1[CH:25]=[CH:24][CH:23]=[C:22]([F:26])[C:19]=1[CH2:20][O:1][C:2]1[CH:10]=[CH:9][C:5]([CH2:6][C:7]#[N:8])=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 265484-Hydroxybenzyl cyanideHCID 5814352-(Bromomethyl)-1,3-difluorobenzene

Produkt 1

HCID 21964471(4-(2,6-Difluorobenzyloxy)phenyl)-acetonitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of 4-Hydroxybenzyl cyanide (5 g, 37.5 mmol) and K2CO3 (6.74 g, 48.8 mmol) in dry DMF (20 ml) was added 2,6-Difluorobenzyl bromide (7.77 g, 37.5 mmol). The reaction mixture was stirred for 4 hours at room temperature and concentrated in vacuo. The crude residue was taken in EtOAc and washed with water and brine. The aqueous layer was washed one more time with EtOAc. The combined organic layers were dried over Na2SO4 filtered, and concentrated to provide the title compound as a white solid.

Aufarbeitung

  1. concentrationconcentrated in vacuo
  2. washwashed with water and brine
  3. washThe aqueous layer was washed one more time with EtOAc
  4. dry with materialThe combined organic layers were dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-fae8d767f9e949d2abdb4e613181892b
Quelldatensatz
uspto-grants-2005_02
Patentnummer
US06858602B2

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