Sulfuric Acid → 2,5-Difluoro-4-nitroaniline

HRID 1033185

Reaktionsgleichung

Reaktionsgleichung von HRID 1033185
CC1C=CC(S([NH:11][C:12]2[CH:17]=[C:16]([F:18])[C:15]([N+:19]([O-:21])=[O:20])=[CH:14][C:13]=2[F:22])(=O)=O)=CC=1.S(=O)(=O)(O)O.[OH-].[NH4+]>O>[F:22][C:13]1[CH:14]=[C:15]([N+:19]([O-:21])=[O:20])[C:16]([F:18])=[CH:17][C:12]=1[NH2:11]

Komponenten

5

Edukt 3

HCID 1118Sulfuric AcidHCID 14923Ammonium HydroxideHCID 22921537N-(4-methylphenylsulfonyl)-2,5-difluoro-4-nitroaniline

Produkt 1

HCID 2359302,5-Difluoro-4-nitroanilineAusbeute 95,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

To a stirred mixture of 12.2 g (0.0370 mole) of N-(4-methylphenylsulfonyl)-2,5-difluoro-4-nitroaniline in 20 ml of water was added 70 ml of concentrated sulfuric acid. This mixture was heated at 90° C. for 15 minutes and then was allowed to cool and stir at room temperature for five days. The reaction mixture was poured into ice-water, and the aqueous mixture was neutralized with concentrated ammonium hydroxide. The resulting solid was collected by filtration. The filter cake was washed with water and was dried under reduced pressure to yield 6.15 g of 2,5-difluoro-4-nitroaniline. The nmr spectrum was consistent with the proposed structure.

Aufarbeitung

  1. temperatureto cool
  2. filtrationThe resulting solid was collected by filtration
  3. washThe filter cake was washed with water
  4. customwas dried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-49dd28249d22453fa276af730e2f294b
Quelldatensatz
uspto-grants-1994_05
Patentnummer
US05310724

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