Water → 6-Ethyl-2-oxo-1-phenyl-1,2-dihydropyridine-3-carboxylic acid

HRID 2095782노트

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HRID 2095782 반응식
[CH2:1]([C:3]1[N:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:7](=[O:15])[C:6]([C:16]#N)=[CH:5][CH:4]=1)[CH3:2].[OH-:18].[Na+].[OH2:20]>S(=O)(=O)(O)O>[CH2:1]([C:3]1[N:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:7](=[O:15])[C:6]([C:16]([OH:20])=[O:18])=[CH:5][CH:4]=1)[CH3:2]

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 669685986-Ethyl-2-oxo-1-phenyl-1,2-dihydropyridine-3-carbonitrile

생성물 1

HCID 581585696-Ethyl-2-oxo-1-phenyl-1,2-dihydropyridine-3-carboxylic acid수율 72%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

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온도
120 °C

실험 절차

6-Ethyl-2-oxo-1-phenyl-1,2-dihydropyridine-3-carbonitrile (395 mg, 1.76 mmol) was dissolved in conc. sulfuric acid (0.4 mL) and water (0.4 mL), and the mixture was stirred with heating at 120° C. for 7 hr. 1N Aqueous sodium hydroxide solution was added to the reaction solution, and the mixture was washed with ethyl acetate. 1N Hydrochloric acid was added to the aqueous layer, and the mixture was extracted 3 times with ethyl acetate. The combined organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and filtered, and the solvent was evaporated under reduced pressure. The residue was washed with ethyl acetate to give the title compound (310 mg, 72%) as a colorless solid.

후처리

  1. washthe mixture was washed with ethyl acetate
  2. addition1N Hydrochloric acid was added to the aqueous layer
  3. extractionthe mixture was extracted 3 times with ethyl acetate
  4. washThe combined organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customthe solvent was evaporated under reduced pressure
  8. washThe residue was washed with ethyl acetate

출처 및 근거

ORD 기록
ord-f5dd924ee3ba496badf11f1d708f9a35
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08445509B2

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