Water → HCID 14986264、化合物

HRID 2248756ノート

反応式

HRID 2248756 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.[C:19]([O:23][CH2:24][C:25](Cl)=[O:26])(=[O:22])[CH2:20][CH3:21].O>C(Cl)Cl>[CH2:11]([NH:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:2]([NH:1][C:25](=[O:26])[CH2:24][O:23][C:19](=[O:22])[CH2:20][CH3:21])[C:3]=1[C:4]#[N:5])[CH3:12]

参加物

6

反応物 4

HCID 962WaterHCID 1049PyridineHCID 11252105Propionyloxyacetyl chlorideHCID 127157182-Amino-6-(ethylamino)benzonitrile

生成物 1

HCID 14986264HCID 14986264、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 (2.3 g) in methylene chloride (50 ml) is added pyridine (1.6 ml), and thereto is added dropwise propionyloxyacetyl chloride (3.0 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 (1.6 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-c037378908494ffbbffa2ae2d5695fcf
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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