Hydrochloric Acid → Ethyl 2-acetylnicotinate

HRID 240412노트

반응식

HRID 240412 반응식
C([O:3][C:4]([C:6]1[N:16]=[CH:15][CH:14]=[CH:13][C:7]=1[C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH2:5])C.Cl>CC(C)=O>[C:4]([C:6]1[N:16]=[CH:15][CH:14]=[CH:13][C:7]=1[C:8]([O:10][CH2:11][CH3:12])=[O:9])(=[O:3])[CH3:5]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 86680868Ethyl 2-(1-ethoxyvinyl)nicotinate

생성물 1

HCID 86680869Ethyl 2-acetylnicotinate수율 63.6%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a mixture of ethyl 2-(1-ethoxyvinyl)nicotinate (27 g) and acetone (300 mL) was added 2M hydrochloric acid (370 mL), and the mixture was stirred overnight at room temperature. The solvent was evaporated under reduced pressure, to the residue were added ethyl acetate and saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (15 g).

후처리

  1. customThe solvent was evaporated under reduced pressure, to the residue
  2. additionwere added ethyl acetate and saturated aqueous sodium hydrogen carbonate solution
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-9533e6323ef54e719dceff54847c207b
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648079B2

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