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

HRID 2248753
ノート
印刷プレビュー

反応式

HRID 2248753 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.[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 149862632-(Methylamino)-6-(phenoxyacetylamino)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 (3.6 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.

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
  5. customThe resulting crude crystals are recrystallized from ethanol

出典と根拠

ORDレコード
ord-64a025258a8842658de7db8e85efeeef
出典データセット
uspto-grants-1991_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05041462

反応ノート

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