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Water → HCID 14986258、化合物

HRID 2248748
ノート
印刷プレビュー

反応式

HRID 2248748 の反応式
[NH2:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([NH:10][CH2:11][CH3:12])[C:3]=1[C:4]#[N:5].N1C=CC=CC=1.[CH3:19][O:20][CH2:21][C:22](Cl)=[O:23].O>C(Cl)Cl>[CH2:11]([NH:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:2]([NH:1][C:22](=[O:23])[CH2:21][O:20][CH3:19])[C:3]=1[C:4]#[N:5])[CH3:12]
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 96623Methoxyacetyl chlorideHCID 127157182-Amino-6-(ethylamino)benzonitrile

生成物 1

HCID 14986258HCID 14986258、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-amino-6-(ethylamino)benzonitrile (3.4 g) in methylene chloride (50 ml) is added pyridine (2.4 ml), and thereto is added dropwise methoxyacetyl chloride (2.8 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
  5. customThe resulting crude crystals are recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-18b3b16242f14763a911f42e841dd28e
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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このページの内容参加物実験手順後処理出典と根拠反応ノート