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

HRID 1030985

반응식

HRID 1030985 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 2359302,5-Difluoro-4-nitroaniline수율 95.5%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
90 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7d8468be17cf41d8a9b17fd06a33e3ff
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05108486

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