Hydrochloric Acid → Ethyl 2-acetylnicotinate

HRID 60613ノート

反応式

HRID 60613 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 86680869Ethyl 2-acetylnicotinate収率 63.6%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-46478a1790a94dacaebc858c4b71ba66
出典データセット
uspto-grants-2016_09
特許番号
US09440990B2

反応ノート

読み込み中…