Hydrazine hydrate (1:1) → HCID 178497263, 화합물

HRID 1178144

반응식

HRID 1178144 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 178497263HCID 178497263, 화합물수율 77.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-249678e1f54b485bb3589580bf01fba9
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07842696B2

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