Acetic Acid → 2,5-difluoro-4-nitro-N-benzenesulphonylaniline

HRID 4235

反応式

HRID 4235 の反応式
C(O)(=O)C.[N:5]([O-:7])=[O:6].[Na+].[F:9][C:10]1[CH:25]=[CH:24][C:23]([F:26])=[CH:22][C:11]=1[NH:12][S:13]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)(=[O:15])=[O:14].[N+]([O-])(O)=O>O>[F:9][C:10]1[CH:25]=[C:24]([N+:5]([O-:7])=[O:6])[C:23]([F:26])=[CH:22][C:11]=1[NH:12][S:13]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)(=[O:14])=[O:15]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 944Nitric AcidHCID 8500589N-(2,5-difluorophenyl)benzenesulfonamideHCID 23668193Sodium Nitrite

生成物 1

HCID 201519862,5-difluoro-4-nitro-N-benzenesulphonylaniline

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
96 °C

実験手順

To 310 ml of acetic acid diluted with 160 ml of water are added: 1.5 g of sodium nitrite, 0.16 mole (42 g) of 2,5-difluoro-N-benzenesulphonylaniline prepared in the previous stage and 0.94 mole (39 ml) of nitric acid (d=1.52). The reaction mixture is heated to 96° C. for 1 hour. After cooling it is poured onto 1 kg of ice and water. The expected product precipitates. After being filtered off and washed to neutrality it is recrystallized from 250 ml of acetic acid; it melts at 176° C.

後処理

  1. additionare added
  2. temperatureAfter cooling it
  3. customThe expected product precipitates
  4. filtrationAfter being filtered off
  5. washwashed
  6. customis recrystallized from 250 ml of acetic acid

出典と根拠

ORDレコード
ord-6690a163904649839ee51f83c59f74e3
出典データセット
uspto-grants-1988_02
特許番号
US04725283

関連ノート

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