Nitric Acid → 2'-Nitro-4'-thiocyano-p-toluenesulfonanilide

HRID 1356673

反応式

HRID 1356673 の反応式
[S:1]([C:4]1[CH:20]=[CH:19][C:7]([NH:8][S:9]([C:12]2[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=2)(=[O:11])=[O:10])=[CH:6][CH:5]=1)[C:2]#[N:3].[N+:21]([O-])([OH:23])=[O:22].O>C(O)(=O)C>[N+:21]([C:6]1[CH:5]=[C:4]([S:1][C:2]#[N:3])[CH:20]=[CH:19][C:7]=1[NH:8][S:9]([C:12]1[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=1)(=[O:11])=[O:10])([O-:23])=[O:22]

参加物

5

反応物 3

HCID 944Nitric AcidHCID 962WaterHCID 8034834-{[(4-Methylphenyl)sulfonyl]amino}phenyl thiocyanate

生成物 1

HCID 185092522'-Nitro-4'-thiocyano-p-toluenesulfonanilide収率 99%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

4′-Thiocyano-p-toluenesulfonanilide (19.2 g (63.2 mmol)) was dissolved in acetic acid (60 ml). To this, fuming nitric acid (3.04 ml (75.9 mmol)) was added dropwise with stirring at room temperature. Then, the mixture was stirred at 50° C. for 4 hours, poured into water, and the crystals separated were filtered and washed with water. The resulting crystals were dissolved in ethyl acetate, and the solution was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to give 21.8 g (99%) of 2′-nitro-4′-thiocyano-p-toluenesulfonanilide as pale yellow crystals.

後処理

  1. stirringThen, the mixture was stirred at 50° C. for 4 hours
  2. customthe crystals separated
  3. filtrationwere filtered
  4. washwashed with water
  5. dissolutionThe resulting crystals were dissolved in ethyl acetate
  6. dry with materialthe solution was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-10eeae91fe154df3aab70945d8b1ac0a
出典データセット
uspto-grants-2003_07
特許番号
US06586617B1

関連ノート

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