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Acetoxyacetyl chloride → HCID 14986274, 화합물

HRID 2248767
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HRID 2248767 반응식
[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]
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참가 물질

4

반응물 2

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

생성물 1

HCID 14986274HCID 14986274, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7024412e01ec476590fadfcc745be884
출처 데이터셋
uspto-grants-1991_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05041462

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