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Acetyl chloride → N-(2-acetyl-5-phenyl-pyrazol-3-yl)acetamide

HRID 1615712
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HRID 1615712 반응식
[C:1]1([C:7]2[NH:11][N:10]=[C:9]([NH2:12])[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CN1[CH2:19][CH2:18][O:17]CC1.[C:20](Cl)(=[O:22])[CH3:21]>C(Cl)Cl.O>[C:20]([N:10]1[C:9]([NH:12][C:18](=[O:17])[CH3:19])=[CH:8][C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[N:11]1)(=[O:22])[CH3:21]
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참가 물질

6

반응물 3

HCID 6367Acetyl chlorideHCID 79724-MethylmorpholineHCID 1366553-Amino-5-phenylpyrazole

생성물 1

HCID 86717295N-(2-acetyl-5-phenyl-pyrazol-3-yl)acetamide수율 88.2%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 5-phenyl-1H-pyrazol-3-amine (18.6 g, 0.117 mol) and N-methylmorpholine (30.8 mL, 0.281 mol) in CH2Cl2 (250 mL) was added acetyl chloride (20 mL, 0.281 mol) dropwise at 0° C. under an atmosphere of nitrogen. The reaction mixture was stirred at room temperature for 3 h. The reaction mixture was diluted with CH2Cl2 and water. The layers were separated and the organic layer was washed with water and brine, dried (phase separator cartridge) and concentrated in vacuo. Diethyl ether was added to the residue and the solid was collected by filtration, yielding the title compound as a solid (25.1 g).

후처리

  1. customThe layers were separated
  2. washthe organic layer was washed with water and brine
  3. customdried (phase separator cartridge)
  4. concentrationconcentrated in vacuo
  5. additionDiethyl ether was added to the residue
  6. filtrationthe solid was collected by filtration

출처 및 근거

ORD 기록
ord-c0b72b16019348b2933449c32e606293
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08765762B2

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