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

HRID 377638
ノート
印刷プレビュー

反応式

HRID 377638 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 7187Benzoyl Peroxide触媒HCID 5943Carbon Tetrachloride
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-97ab40c8b566468d93deee4bf08d21a8
出典データセット
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06028084

反応ノート

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