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Phosphorus oxychloride → 2',4'-Dicyano-p-toluenesulfonanilide

HRID 1356653
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HRID 1356653 반응식
P(Cl)(Cl)(Cl)=O.[C:6]([C:9]1[CH:25]=[C:24]([C:26](=O)[NH2:27])[CH:23]=[CH:22][C:10]=1[NH:11][S:12]([C:15]1[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][CH:16]=1)(=[O:14])=[O:13])(=O)[NH2:7]>O>[C:6]([C:9]1[CH:25]=[C:24]([C:26]#[N:27])[CH:23]=[CH:22][C:10]=1[NH:11][S:12]([C:15]1[CH:16]=[CH:17][C:18]([CH3:21])=[CH:19][CH:20]=1)(=[O:14])=[O:13])#[N:7]
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참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 18509262HCID 18509262, 화합물

생성물 1

HCID 185093212',4'-Dicyano-p-toluenesulfonanilide수율 60%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

Phosphorus oxychloride (5.00 g) was added to 2′,4′-dicarbamoyl-p-toluenesulfonanilide (0.30 g (0.90 mmol), and the mixture was heated at 50° C. for 4 hours with stirring. After cooling, addition of water, and stirring brought about precipitation of an insoluble solid. These crystals were filtered, washed with water and recrystallized from ethyl acetate-hexane to give 0.16 g (60%) of 2′,4′-dicyano-p-toluenesulfonanilide as pale brown crystals.

후처리

  1. temperatureAfter cooling
  2. stirringstirring
  3. custombrought about precipitation of an insoluble solid
  4. filtrationThese crystals were filtered
  5. washwashed with water
  6. customrecrystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-ba6d7025796645d0b29ddd3b82254cb3
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06586617B1

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