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

HRID 1033185

反応式

HRID 1033185 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 2359302,5-Difluoro-4-nitroaniline収率 95.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-49dd28249d22453fa276af730e2f294b
出典データセット
uspto-grants-1994_05
特許番号
US05310724

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