Nitric Acid → 1-Chloro-2-fluoro-4-nitro-5-(trifluoromethyl)benzene

HRID 2417698

Reaktionsgleichung

Reaktionsgleichung von HRID 2417698
[N+:1]([O-:4])(O)=[O:2].[Cl:5][C:6]1[CH:7]=[C:8]([C:13]([F:16])([F:15])[F:14])[CH:9]=[CH:10][C:11]=1[F:12]>>[Cl:5][C:6]1[C:11]([F:12])=[CH:10][C:9]([N+:1]([O-:4])=[O:2])=[C:8]([C:13]([F:14])([F:15])[F:16])[CH:7]=1

Komponenten

3

Edukt 2

HCID 944Nitric AcidHCID 157153Benzene, 2-chloro-1-fluoro-4-(trifluoromethyl)-

Produkt 1

HCID 201633061-Chloro-2-fluoro-4-nitro-5-(trifluoromethyl)benzene

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

About 500 parts of aqueous nitric acid was added slowly, with stirring, to a reaction vessel containing about 400 parts of 3-chloro-4-fluorobenzotrifluoride. The temperature of the reaction mixture was maintained at about 40° C. during the addition, then raised to about 60° C. and maintained thereat for about 5 hours. The reaction mixture was allowed to settle. The aqueous layer was removed and the organic layer was washed twice with 500 parts of water, treated several times with a saturated solution of sodium bicarbonate, washed with water again, dried over anhydrous magnesium sulfate, and filtered. The filtrate was distilled at reduced pressure to yield 347 parts of 5-chloro-4-fluoro-2-nitrobenzotrifluoride.

Aufarbeitung

  1. temperatureraised to about 60° C.
  2. temperaturemaintained
  3. customThe aqueous layer was removed
  4. washthe organic layer was washed twice with 500 parts of water
  5. additiontreated several times with a saturated solution of sodium bicarbonate
  6. washwashed with water again
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. distillationThe filtrate was distilled at reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-d5e5dea3eb8046218951f189f2a249a1
Quelldatensatz
uspto-grants-1984_09
Patentnummer
US04469893

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