4-Fluorophenylhydrazine hydrochloride → HCID 19886090、化合物

HRID 654777ノート

反応式

HRID 654777 の反応式
[C:1]1([CH3:17])[CH:6]=[CH:5][C:4]([C:7](=O)[CH2:8][C:9](=O)[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:3][CH:2]=1.Cl.[F:19][C:20]1[CH:25]=[CH:24][C:23]([NH:26][NH2:27])=[CH:22][CH:21]=1>O1CCOCC1.C(O)C>[F:19][C:20]1[CH:25]=[CH:24][C:23]([N:26]2[C:7]([C:4]3[CH:5]=[CH:6][C:1]([CH3:17])=[CH:2][CH:3]=3)=[CH:8][C:9]([C:10]([O:12][CH2:13][CH3:14])=[O:11])=[N:27]2)=[CH:22][CH:21]=1

参加物

5

反応物 2

HCID 699814-Fluorophenylhydrazine hydrochlorideHCID 595052Ethyl 2,4-dioxo-4-(p-tolyl)butanoate

生成物 1

HCID 19886090HCID 19886090、化合物収率 41.5%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

A mixture of ethyl 4-(4-tolyl)-2,4-dioxobutanoate (4.7 g) and 4-fluorophenylhydrazine hydrochloride (3.6 g) in dioxane (35 ml) and ethanol (35 ml) was refluxed for 5 hours. The mixture was filtered and the filtrate was concentrated in vacuo. The oily residue (8 g) was purified.by column chromatography on silica gel (130 g) eluting with chloroform to give an oil of ethyl 1-(4-fluorophenyl)-5-(4-tolyl)pyrazole-3-carboxylate (2.7 g).

後処理

  1. temperaturewas refluxed for 5 hours
  2. filtrationThe mixture was filtered
  3. concentrationthe filtrate was concentrated in vacuo
  4. washeluting with chloroform

出典と根拠

ORDレコード
ord-e9c98eacbb4a4fa49693d26d9df75d47
出典データセット
uspto-grants-1992_07
特許番号
US05134142

反応ノート

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