Water → 2-(Ethoxyacetylamino)-6-(methylamino)benzonitrile

HRID 2248751노트

반응식

HRID 2248751 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.[CH2:18]([O:20][CH2:21][C:22](Cl)=[O:23])[CH3:19].O>C(Cl)Cl>[CH2:18]([O:20][CH2:21][C:22]([NH:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([NH:10][CH3:11])[C:3]=1[C:4]#[N:5])=[O:23])[CH3:19]

참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 84189Ethoxyacetyl chlorideHCID 127157172-Amino-6-(methylamino)benzonitrile

생성물 1

HCID 149862612-(Ethoxyacetylamino)-6-(methylamino)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 (3.9 ml), and thereto is added dropwise ethoxyacetyl chloride (5 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 ethyl acetate-hexane to give the title compound (3.2 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 The resulting crude crystals
  5. customare recrystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-444b27a8709145919be95f4c2e62fd23
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05041462

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