Dimethylformamide → 1,3-Dichloro-2-fluoro-5-nitrobenzene

HRID 1709691

Reaktionsgleichung

Reaktionsgleichung von HRID 1709691
[Cl:1][C:2]1[CH:3]=[C:4]([N+:10]([O-:12])=[O:11])[CH:5]=[C:6]([Cl:9])[C:7]=1Cl.[F-:13].[K+].CN(C)C=O>O>[Cl:1][C:2]1[CH:3]=[C:4]([N+:10]([O-:12])=[O:11])[CH:5]=[C:6]([Cl:9])[C:7]=1[F:13]

Komponenten

5

Edukt 3

HCID 6228DimethylformamideHCID 883653,4,5-TrichloronitrobenzeneHCID 522689Potassium Fluoride2×

Produkt 1

HCID 765541,3-Dichloro-2-fluoro-5-nitrobenzene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 3,4,5-trichloronitrobenzene (13.55 g, 59 mmol), potassium fluoride (4.65 g, 80 mmol) and dimethylformamide (DMF; 66 ml) is heated at 140° for 15 hours. An additional 2.5 g of potassium fluoride is added and the mixture is stirred an additional 15 hours at 140°. The reaction mixture is poured into water and extracted with ether. The combined organic layers are washed with water and with brine and filtered, and the solvent is removed to give a dark solid, which is purified by column chromatography to give 3,5-dichloro-4-fluoronitrobenzene, a yellow powder.

Aufarbeitung

  1. temperatureis heated at 140° for 15 hours
  2. extractionextracted with ether
  3. washThe combined organic layers are washed with water and with brine
  4. filtrationfiltered
  5. customthe solvent is removed
  6. customto give a dark solid, which
  7. customis purified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-3a22b09c30b14d1b975aac63b5bfbd61
Quelldatensatz
uspto-grants-1990_08
Patentnummer
US04950678

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