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Water → 2-(Methylamino)-6-(phenoxyacetylamino)benzonitrile

HRID 2248753
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HRID 2248753 반응식
[NH2:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([NH:10][CH3:11])[C:3]=1[C:4]#[N:5].N1C=CC=CC=1.[O:18]([CH2:25][C:26](Cl)=[O:27])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.O>C(Cl)Cl>[CH3:11][NH:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:2]([NH:1][C:26](=[O:27])[CH2:25][O:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:3]=1[C:4]#[N:5]
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참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 69703Phenoxyacetyl chlorideHCID 127157172-Amino-6-(methylamino)benzonitrile

생성물 1

HCID 149862632-(Methylamino)-6-(phenoxyacetylamino)benzonitrile

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 2-amino-6-(methylamino)benzonitrile (3.3 g) in methylene chloride (50 ml) is added pyridine (3.6 ml), and thereto is added dropwise phenoxyacetyl chloride (6.2 ml) which is cooled in an ice bath. The mixture is stirred at room temperature for 1 hour, and thereafter, water is added thereto, and the mixture is extracted with methylene chloride. The organic layer is dried over anhydrous sodium sulfate, and the solvent is distilled off under reduced pressure. The resulting crude crystals are recrystallized from ethanol to give the title compound (1.4 g) having the following physical properties.

후처리

  1. temperatureis cooled in an ice bath
  2. extractionthe mixture is extracted with methylene chloride
  3. dry with materialThe organic layer is dried over anhydrous sodium sulfate
  4. distillationthe solvent is distilled off under reduced pressure
  5. customThe resulting crude crystals are recrystallized from ethanol

출처 및 근거

ORD 기록
ord-64a025258a8842658de7db8e85efeeef
출처 데이터셋
uspto-grants-1991_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05041462

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