Water → 4-{[(4-Methylphenyl)sulfonyl]amino}phenyl thiocyanate

HRID 1356672

反応式

HRID 1356672 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][C:9]#[N:10])=[CH:4][CH:3]=1.[C:11]1([CH3:21])[CH:16]=[CH:15][C:14]([S:17](Cl)(=[O:19])=[O:18])=[CH:13][CH:12]=1.O>N1C=CC=CC=1>[S:8]([C:5]1[CH:6]=[CH:7][C:2]([NH:1][S:17]([C:14]2[CH:15]=[CH:16][C:11]([CH3:21])=[CH:12][CH:13]=2)(=[O:19])=[O:18])=[CH:3][CH:4]=1)[C:9]#[N:10]

参加物

5

反応物 3

HCID 962WaterHCID 73974-Toluenesulfonyl chlorideHCID 76336[(4-Aminophenyl)sulfanyl]formonitrile

生成物 1

HCID 8034834-{[(4-Methylphenyl)sulfonyl]amino}phenyl thiocyanate収率 98%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 4-Aminophenyl thiocyanate (10.0 g (66.6 mmol)) in pyridine (70 ml), p-toluenesulfonyl chloride (12.7 g (66.6 mmol)) was added with stirring at room temperature, and the mixture was stirred at room temperature for 16 hours. Then, water was added to the reaction mixture and the resulting mixture was extracted with ethyl acetate. The extract was washed with dilute hydrochloric acid and a saturated aqueous solution of sodium chloride, dried over magnesium sulfate, filtered and concentrated under reduced pressure to give 19.4 g (98%) of 4′-thiocyano-p-toluenesulfonanilide as pale yellow crystals.

後処理

  1. stirringthe mixture was stirred at room temperature for 16 hours
  2. extractionthe resulting mixture was extracted with ethyl acetate
  3. washThe extract was washed with dilute hydrochloric acid
  4. dry with materiala saturated aqueous solution of sodium chloride, dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-2506627016cf4c9f849692e0a60c3e4b
出典データセット
uspto-grants-2003_07
特許番号
US06586617B1

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