Hydrazine hydrate (1:1) → HCID 178497263、化合物

HRID 1178144

反応式

HRID 1178144 の反応式
[NH2:1][NH2:2].O.[CH2:4]([O:6][C:7](=[O:19])[C:8](=O)[CH2:9][C:10](=O)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)C>CO>[CH3:4][O:6][C:7]([C:8]1[CH:9]=[C:10]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[NH:2][N:1]=1)=[O:19]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 2265032,4-Dioxo-4-phenyl-butyric acid ethyl ester

生成物 1

HCID 178497263HCID 178497263、化合物収率 77.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

NH2—NH2—H2O (1.0 g, 20 mmol) was added to a solution of 2,4-dioxo-4-phenyl-butyric acid ethyl ester (1.94 g, 8.81 mmol) in methanol (17 mL). The resulting reaction mixture was heated to reflux for two and half hours. The methanol was evaporated and the resulting solid was heated with 2.5% ethyl acetate in hexane to afford 5-phenyl-1H-pyrazole-3-carboxylic acid methyl ester as a solid in 77.3% yield. LC-MS purity: 93.345%.

後処理

  1. customThe resulting reaction mixture
  2. temperaturewas heated
  3. temperatureto reflux for two and half hours
  4. customThe methanol was evaporated
  5. temperaturethe resulting solid was heated with 2.5% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-249678e1f54b485bb3589580bf01fba9
出典データセット
uspto-grants-2010_11
特許番号
US07842696B2

関連ノート

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