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

HRID 2248751ノート

反応式

HRID 2248751 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 149862612-(Ethoxyacetylamino)-6-(methylamino)benzonitrile

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-444b27a8709145919be95f4c2e62fd23
出典データセット
uspto-grants-1991_08
特許番号
US05041462

反応ノート

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