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

HRID 1356672

반응식

HRID 1356672 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2506627016cf4c9f849692e0a60c3e4b
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06586617B1

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