Benzene → 4-(2,4-Dichlorobenzoyl)-1-methyl-5-(p-acetylbenzyloxy)pyrazole

HRID 637595

反応式

HRID 637595 の反応式
C1C=CC=CC=1.[Cl:7][C:8]1[CH:22]=[C:21]([Cl:23])[CH:20]=[CH:19][C:9]=1[C:10]([C:12]1[CH:13]=[N:14][N:15]([CH3:18])[C:16]=1[OH:17])=[O:11].[C:24]([C:27]1[CH:34]=[CH:33][C:30]([CH2:31]Br)=[CH:29][CH:28]=1)(=[O:26])[CH3:25]>C(N(CC)CC)C>[Cl:7][C:8]1[CH:22]=[C:21]([Cl:23])[CH:20]=[CH:19][C:9]=1[C:10]([C:12]1[CH:13]=[N:14][N:15]([CH3:18])[C:16]=1[O:17][CH2:31][C:30]1[CH:33]=[CH:34][C:27]([C:24](=[O:26])[CH3:25])=[CH:28][CH:29]=1)=[O:11]

参加物

5

反応物 3

HCID 241BenzeneHCID 5837851-[4-(Bromomethyl)phenyl]ethan-1-oneHCID 178481842HCID 178481842、化合物

生成物 1

HCID 155907284-(2,4-Dichlorobenzoyl)-1-methyl-5-(p-acetylbenzyloxy)pyrazole収率 83%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

In 30 ml of dry benzene containing 0.50 g (0.005 mol) of triethylamine was dissolved 1.36 (0.005 mol) of 4-(2,4-dichlorobenzoyl)-1-methyl-5-hydroxypyrazole, and then 1.07 g (0.005 mol) of p-acetylbenzylbromide was added thereto. The resulting mixture was heated under reflux for 3 hours. After cooling the reaction mixture, the salt precipitated was filtered off and the solvent was distilled off therefrom under reduced pressure. The resulting oil was purified through column chromatography on silica gel using benzene/ethyl acetate 8:1 as an eluent to give 1.67 g of the title compound (yield 83%).

後処理

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for 3 hours
  3. temperatureAfter cooling the reaction mixture
  4. customthe salt precipitated
  5. filtrationwas filtered off
  6. distillationthe solvent was distilled off
  7. customThe resulting oil was purified through column chromatography on silica gel

出典と根拠

ORDレコード
ord-70c3c8650efc4dc0acd3abc0a8cb70b0
出典データセット
uspto-grants-1985_12
特許番号
US04557753

関連ノート

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