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Benzoylacetone → 1-(4-Methoxyphenyl)-3-methyl-5-phenyl-1H-pyrazole

HRID 903936
ノート
印刷プレビュー

反応式

HRID 903936 の反応式
Cl.[CH3:2][O:3][C:4]1[CH:9]=[CH:8][C:7]([NH:10][NH2:11])=[CH:6][CH:5]=1.[C:12]1([C:18](=O)[CH2:19][C:20](=O)[CH3:21])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH3:2][O:3][C:4]1[CH:9]=[CH:8][C:7]([N:10]2[C:18]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[CH:19][C:20]([CH3:21])=[N:11]2)=[CH:6][CH:5]=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 3

HCID 7166BenzoylacetoneHCID 11430Potassium CarbonateHCID 27239044-Methoxyphenylhydrazine hydrochloride

生成物 1

HCID 112655551-(4-Methoxyphenyl)-3-methyl-5-phenyl-1H-pyrazole収率 53%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 8.7 parts of (4-methoxyphenyl)hydrazine hydrochloride, 8.1 parts of 1-phenyl-1,3-butanedione, 7 parts of potassium carbonate and 160 parts of ethanol is stirred and refluxed for 20 hours. The reaction mixture is cooled and poured onto water. The product is extracted twice with 2,2'-oxybispropane. The combined extracts are washed with water, dried, filtered and evaporated. The residue is crystallized twice from petroleumether. The product is filtered off and dried, yielding 7 parts (53%) of 1-(4-methoxyphenyl)-3-methyl-5phenyl-1H-pyrazole; mp. 110° C.

後処理

  1. temperaturerefluxed for 20 hours
  2. temperatureThe reaction mixture is cooled
  3. additionpoured onto water
  4. extractionThe product is extracted twice with 2,2'-oxybispropane
  5. washThe combined extracts are washed with water
  6. customdried
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue is crystallized twice from petroleumether
  10. filtrationThe product is filtered off
  11. customdried

出典と根拠

ORDレコード
ord-853b5670b25a486ab89127472d1226bd
出典データセット
uspto-grants-1980_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04229460

反応ノート

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