Water → 6-Methyl-2-nitrophenylpyruvic acid

HRID 1953851

반응식

HRID 1953851 반응식
[Na].[N+:2]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:6]=1[CH3:12])([O-:4])=[O:3].[C:13](OCC)(=[O:19])[C:14]([O:16]CC)=[O:15].O>C(O)C>[CH3:11][C:7]1[CH:8]=[CH:9][CH:10]=[C:5]([N+:2]([O-:4])=[O:3])[C:6]=1[CH2:12][C:13](=[O:19])[C:14]([OH:16])=[O:15]

참가 물질

6

반응물 4

HCID 962WaterHCID 67391,2-Dimethyl-3-nitrobenzeneHCID 7268Diethyl OxalateHCID 5360545Sodium

생성물 1

HCID 211942326-Methyl-2-nitrophenylpyruvic acid수율 94.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Sodium metal (3.80 g, 165 mmol) was dissolved in absolute ethanol (66 mL) at 0° C. The 3-nitro-o-xylene (10 g, 66.2 mmol) and diethyl oxalate (18 mL, 132 mmol) were then added and the reaction was warmed to room temperature and stirred for 18 hours. The reaction was refluxed for 30 minutes, then cooled and water (22 mL) was added and the reaction was stirred at room temperature for one hour. The reaction was concentrated to remove the ethanol, then extracted with ethyl acetate, washed with brine, dried over sodium sulfate, filtered and concentrated to provide the desired product (13.92 g, 94%).

후처리

  1. temperatureThe reaction was refluxed for 30 minutes
  2. temperaturecooled
  3. stirringthe reaction was stirred at room temperature for one hour
  4. concentrationThe reaction was concentrated
  5. customto remove the ethanol
  6. extractionextracted with ethyl acetate
  7. washwashed with brine
  8. dry with materialdried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated

출처 및 근거

ORD 기록
ord-99e359eefa6243b5908a714353b47a5f
출처 데이터셋
uspto-grants-2000_09
특허 번호
US06117885

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