Acetic Acid → Mls002703379

HRID 484784ノート

反応式

HRID 484784 の反応式
[C:1]1([CH3:19])[CH:6]=[CH:5][C:4]([S:7]([NH:10][C:11]2[C:16]([CH3:17])=[CH:15][CH:14]=[CH:13][C:12]=2[CH3:18])(=[O:9])=[O:8])=[CH:3][CH:2]=1.[N+:20]([O-])([OH:22])=[O:21].C(O)(=O)C.N([O-])=O.[Na+]>O>[C:1]1([CH3:19])[CH:2]=[CH:3][C:4]([S:7]([NH:10][C:11]2[C:16]([CH3:17])=[CH:15][C:14]([N+:20]([O-:22])=[O:21])=[CH:13][C:12]=2[CH3:18])(=[O:8])=[O:9])=[CH:5][CH:6]=1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 944Nitric AcidHCID 262999N-(2,6-dimethylphenyl)-4-methylbenzenesulfonamideHCID 23668193Sodium Nitrite

生成物 1

HCID 263000Mls002703379

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

The sulfonamide intermediate of Example 4 (6.9 g, 0.025 mole) was added to a solution of 6.3 ml of concentrated nitric acid in 50 ml of water, followed by addition of 50 ml of glacial acetic acid and 0.18 g of sodium nitrite. The mixture was heated at reflux for one hour, then poured into 100 ml of water. The crude product thus isolated was recrystallized from ethanol to give 6.5 g of the title compound. Structure assignment was supported by the nmr spectrum and by elemental analysis.

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for one hour
  3. customThe crude product thus isolated
  4. customwas recrystallized from ethanol

出典と根拠

ORDレコード
ord-608ef35de8e148e19da0a0f8ad804523
出典データセット
uspto-grants-1985_08
特許番号
US04533739

反応ノート

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