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

HRID 2258618ノート

反応式

HRID 2258618 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>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

4

反応物 2

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

生成物 1

HCID 2359302,5-Difluoro-4-nitroaniline収率 143.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

A stirred solution of 25.0 grams (0.076 mole) of N-(4-methylphenylsulfonyl)-2,5-difluoro-4-nitroaniline in 50 mL of water was cooled in an ice-water bath, and 150 mL of concentrated sulfuric acid was carefully added portionwise. Upon completion of the addition, the reaction mixture was heated to about 90° C., where it stirred for about four hours. The reaction mixture was then cooled and poured into wet ice. The resultant solid was collected by filtration and dried, yielding about 19.0 grams of 2,5-difluoro-4-nitroaniline. The NMR spectrum was consistent with the proposed structure.

後処理

  1. additionUpon completion of the addition
  2. temperatureThe reaction mixture was then cooled
  3. additionpoured into wet ice
  4. filtrationThe resultant solid was collected by filtration
  5. customdried

出典と根拠

ORDレコード
ord-6e62b75be3694c899a13ab85019d3e76
出典データセット
uspto-grants-1997_08
特許番号
US05661108

反応ノート

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