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N-bromobutanimide → Ethyl 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-bromomethylpyrazole-3-carboxylate

HRID 377638
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HRID 377638 반응식
[Br:1]N1C(=O)CCC1=O.[Cl:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[N:20]([C:21]3[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:22]=3[Cl:28])[N:19]=[C:18]([C:29]([O:31][CH2:32][CH3:33])=[O:30])[C:17]=2[CH3:34])=[CH:12][CH:11]=1>C(Cl)(Cl)(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Cl:9][C:10]1[CH:11]=[CH:12][C:13]([C:16]2[N:20]([C:21]3[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:22]=3[Cl:28])[N:19]=[C:18]([C:29]([O:31][CH2:32][CH3:33])=[O:30])[C:17]=2[CH2:34][Br:1])=[CH:14][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 67184N-bromobutanimideHCID 10938462Ethyl 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methyl-1H-pyrazole-3-carboxylate

생성물 1

HCID 19356248Ethyl 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-bromomethylpyrazole-3-carboxylate수율 110.4%

시약·촉매·용매 2

HCID 7187Benzoyl Peroxide촉매HCID 5943Carbon Tetrachloride
용매

실험 절차

4.8 g of N-bromosuccinimide and 20 mg of benzoyl peroxide are added to a solution of 10.73 g of ethyl 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methylpyrazole-3-carboxylate in 200 ml of CCl4 and the mixture is then refluxed for 16 hours. The insoluble material is filtered off and the filtrate is concentrated under vacuum. The residue is extracted with DCM, the organic phase is washed with water and dried over MgSO4 and the solvent is evaporated off under vacuum to give 14.13 g of the expected product.

후처리

  1. temperaturethe mixture is then refluxed for 16 hours
  2. filtrationThe insoluble material is filtered off
  3. concentrationthe filtrate is concentrated under vacuum
  4. extractionThe residue is extracted with DCM
  5. washthe organic phase is washed with water
  6. dry with materialdried over MgSO4
  7. customthe solvent is evaporated off under vacuum

출처 및 근거

ORD 기록
ord-97ab40c8b566468d93deee4bf08d21a8
출처 데이터셋
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06028084

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