Dimethylformamide → 3-(2-Fluoro-4-nitrophenoxy)pyridine

HRID 13233

Reaktionsgleichung

Reaktionsgleichung von HRID 13233
[OH:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O.[F:19][C:20]1[CH:21]=[C:22]([N+:27]([O-:29])=[O:28])[CH:23]=[CH:24][C:25]=1F>C(OCC)(=O)C>[F:19][C:20]1[CH:21]=[C:22]([N+:27]([O-:29])=[O:28])[CH:23]=[CH:24][C:25]=1[O:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 79713-HydroxypyridineHCID 11430Potassium CarbonateHCID 1230531,2-Difluoro-4-nitrobenzene

Produkt 1

HCID 231451003-(2-Fluoro-4-nitrophenoxy)pyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

2.09 g of 3-hydroxypyridine and 5.52 g of potassium carbonate were added to a dimethylformamide (20 ml) solution of 3.18 g of 3,4-difluoronitrobenzene, and the reaction liquid was stirred at 90° C. for 1 hour. The reaction liquid was diluted with ethyl acetate, washed with water and saturated saline in order, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=9/1) to obtain the entitled compound.

Aufarbeitung

  1. customthe reaction liquid
  2. customThe reaction liquid
  3. washwashed with water and saturated saline in order
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customThe solvent was evaporated away under reduced pressure
  6. customthe resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=9/1)
  7. customto obtain the entitled compound

Quellen und Nachweise

ORD-Eintrag
ord-ae345408704b4fb4b3c1225ccec86d21
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07728025B2

Verknüpfte Notizen

Wird geladen…