Lithium Carbonate → HCID 10516707, Verbindung

HRID 1596703

Reaktionsgleichung

Reaktionsgleichung von HRID 1596703
[OH:1][C:2]1[CH:3]=[C:4]([C:9](=[O:11])[CH3:10])[CH:5]=[CH:6][C:7]=1[OH:8].C(=O)([O-])[O-].[Li+].[Li+].Br[CH2:19][C:20]1[C:25]([F:26])=[CH:24][CH:23]=[CH:22][C:21]=1[F:27]>CN(C)C=O>[OH:1][C:2]1[CH:3]=[C:4]([C:9](=[O:11])[CH3:10])[CH:5]=[CH:6][C:7]=1[O:8][CH2:19][C:20]1[C:25]([F:26])=[CH:24][CH:23]=[CH:22][C:21]=1[F:27]

Komponenten

5

Edukt 3

HCID 11125Lithium CarbonateHCID 145303',4'-DihydroxyacetophenoneHCID 5814352-(Bromomethyl)-1,3-difluorobenzene

Produkt 1

HCID 10516707HCID 10516707, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of 3′,4′-dihydroxyacetophenone (25.0 g, 164.3 mmol), lithium carbonate (12.1 g, 164.3 mmol), and α-bromo-2,6-difluorotoluene (34.0 g, 164.3 mmol) in dimethyl formamide (400 mL) is stirred at room temperature for 2 days. The mixture is then filtered through celite, and the filtrate is concentrated in vacuo. The residue is diluted with H2O(200 mL), and the mixture is filtered. The collected solid is recrystallized from ethanol to give 3′-hydroxy-4′-(2,6-difluorobenzyloxy)-acetophenone.

Aufarbeitung

  1. filtrationThe mixture is then filtered through celite
  2. concentrationthe filtrate is concentrated in vacuo
  3. additionThe residue is diluted with H2O(200 mL)
  4. filtrationthe mixture is filtered
  5. customThe collected solid is recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-4f90ac559ab447b1b1a32448c16bb731
Quelldatensatz
uspto-grants-2001_09
Patentnummer
US06291530B1

Verknüpfte Notizen

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