Pyridine → 2',6'-Dinitro-4'-trifluoromethyl-2,2,2-trifluoroacetanilide

HRID 1576377

Reaktionsgleichung

Reaktionsgleichung von HRID 1576377
[N+:1]([C:4]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[C:7]([N+:15]([O-:17])=[O:16])[C:5]=1[NH2:6])([O-:3])=[O:2].N1C=CC=CC=1.[F:24][C:25]([F:30])([F:29])[C:26](Cl)=[O:27].FC(F)(F)C(O)=O>C(O)C>[N+:1]([C:4]1[CH:10]=[C:9]([C:11]([F:12])([F:13])[F:14])[CH:8]=[C:7]([N+:15]([O-:17])=[O:16])[C:5]=1[NH:6][C:26](=[O:27])[C:25]([F:30])([F:29])[F:24])([O-:3])=[O:2]

Komponenten

6

Edukt 4

HCID 1049PyridineHCID 6422Trifluoroacetic acidHCID 99362,6-Dinitro-4-(trifluoromethyl)anilineHCID 61106Trifluoroacetyl chloride

Produkt 1

HCID 215124262',6'-Dinitro-4'-trifluoromethyl-2,2,2-trifluoroacetanilide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 25.1 g. of 2,6-dinitro-4-trifluoromethylaniline in 100 ml. of pyridine was treated with trifluoroacetyl chloride, which has been prepared from 10 ml. of trifluoroacetic acid. Ethanol was added to the resulting mixture until it was homogeneous, and the reaction mixture was then evaporated under vacuum. The residue after evaporation was washed with water, dried, dissolved in acetone, and filtered. Chloroform was added to the filtrate until the product precipitated. The precipitate was separated by filtration and dried to obtain the purified intermediate, 2',6'-dinitro-4'-trifluoromethyl-2,2,2-trifluoroacetanilide.

Aufarbeitung

  1. customhas been prepared from 10 ml
  2. customthe reaction mixture was then evaporated under vacuum
  3. customThe residue after evaporation
  4. washwas washed with water
  5. customdried
  6. dissolutiondissolved in acetone
  7. filtrationfiltered
  8. additionChloroform was added to the filtrate until the product
  9. customprecipitated
  10. customThe precipitate was separated by filtration
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-2acf227a1cfb4dcdbbbcc2e56b5f5bcc
Quelldatensatz
uspto-grants-1976_09
Patentnummer
US03980784

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