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Acetoxyacetyl chloride → HCID 14986274、化合物

HRID 2248767
ノート
印刷プレビュー

反応式

HRID 2248767 の反応式
[NH2:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([N:10]2[CH2:15][CH2:14][O:13][CH2:12][CH2:11]2)[C:3]=1[C:4]#[N:5].[C:16]([O:19][CH2:20][C:21](Cl)=[O:22])(=[O:18])[CH3:17]>N1C=CC=CC=1>[C:16]([O:19][CH2:20][C:21]([NH:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([N:10]2[CH2:11][CH2:12][O:13][CH2:14][CH2:15]2)[C:3]=1[C:4]#[N:5])=[O:22])(=[O:18])[CH3:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 26297Acetoxyacetyl chlorideHCID 127157272-Amino-6-(morpholin-4-yl)benzonitrile

生成物 1

HCID 14986274HCID 14986274、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 2-amino-6-morpholinobenzonitrile (5.6 g) in pyridine (15 ml) is added dropwise acetoxyacetyl chloride (3.3 ml) which is cooled in an ice bath. The mixture is stirred at room temperature for 1 hour, and thereafter, pyridine is distilled off under reduced pressure and thereto is added water, 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 residue is recrystallized from ethanol-toluene-water to give the title compound (4.7 g) having the following physical properties.

後処理

  1. temperatureis cooled in an ice bath
  2. distillationpyridine is distilled off under reduced pressure
  3. additionis added water
  4. extractionthe mixture is extracted with methylene chloride
  5. dry with materialThe organic layer is dried over anhydrous sodium sulfate
  6. distillationthe solvent is distilled off under reduced pressure
  7. customThe resulting residue is recrystallized from ethanol-toluene-water

出典と根拠

ORDレコード
ord-7024412e01ec476590fadfcc745be884
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