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Oxalyl chloride → 4-(3,5-Dimethylpyrazol-1-yl)benzoyl chloride

HRID 1635851
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HRID 1635851 반응식
[CH3:1][C:2]1[CH:6]=[C:5]([CH3:7])[N:4]([C:8]2[CH:16]=[CH:15][C:11]([C:12](O)=[O:13])=[CH:10][CH:9]=2)[N:3]=1.C(Cl)(=O)C([Cl:20])=O>ClCCl.CN(C)C=O>[CH3:1][C:2]1[CH:6]=[C:5]([CH3:7])[N:4]([C:8]2[CH:16]=[CH:15][C:11]([C:12]([Cl:20])=[O:13])=[CH:10][CH:9]=2)[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 65578Oxalyl chlorideHCID 6932064-(3,5-dimethyl-1H-pyrazol-1-yl)benzoic acid

생성물 1

HCID 128534534-(3,5-Dimethylpyrazol-1-yl)benzoyl chloride수율 55%

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 6344Dichloromethane용매

실험 절차

To a suspension of 4-(3,5-dimethylpyrazol-1-yl)benzoic acid (1.34 g) in dichloromethane (25 ml) was added oxalyl chloride (1.0 g) and one drop of dimethylformamide. The mixture was stirred at room temperature for 18 hours and the volatile material was removed under reduced pressure. The residue was dissolved in hexane and filtered through diatomaceous earth. Evaporation of the solvent in vacuo yielded 4-(3,5-dimethylpyrazol-1-yl)benzoyl chloride (0.80 g), which was used without further purification.

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후처리

  1. customthe volatile material was removed under reduced pressure
  2. dissolutionThe residue was dissolved in hexane
  3. filtrationfiltered through diatomaceous earth
  4. customEvaporation of the solvent in vacuo

출처 및 근거

ORD 기록
ord-716a29b4c8644d149d8b3b1dc57f0d61
출처 데이터셋
uspto-grants-2003_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06511974B1

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