Pyrazole → 1-Phenyl-2-(1H-pyrazol-1-yl)ethanone

HRID 133474

반응식

HRID 133474 반응식
Cl[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:4].[NH:11]1[CH:15]=[CH:14][CH:13]=[N:12]1.C([O-])([O-])=O.[K+].[K+]>CC#N.CCOC(C)=O>[C:5]1([C:3](=[O:4])[CH2:2][N:11]2[CH:15]=[CH:14][CH:13]=[N:12]2)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

참가 물질

6

반응물 3

HCID 1048PyrazoleHCID 107572-ChloroacetophenoneHCID 11430Potassium Carbonate

생성물 1

HCID 27663751-Phenyl-2-(1H-pyrazol-1-yl)ethanone

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 1.5 g (9.7 mmol) of 2-chloroacetophenone in 10 mL of MeCN, 0.7 g (10.3 mmol) of pyrazole was added. After all the solids dissolved, 1.4 g (10.1 mmol) of ground K2CO3 was added and the mixture was stirred for 5 h. The reaction was diluted with EtOAc, filtered, and the solid was washed with EtOAc. The filtrate was washed with water and brine, then was dried and concentrated. The residue was chromatographed on a flash column using a gradient of 10-50% EtOAc-hexane to isolate desired product.

후처리

  1. dissolutionAfter all the solids dissolved
  2. filtrationfiltered
  3. washthe solid was washed with EtOAc
  4. washThe filtrate was washed with water and brine
  5. customwas dried
  6. concentrationconcentrated
  7. customThe residue was chromatographed on a flash column

출처 및 근거

ORD 기록
ord-1eabe1ca28e24df185018b6299bd77d2
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07390835B2

연결된 노트

불러오는 중…