反応 #67989

ord-550d0306c7964def8c9e5963eb868381

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added
  2. 2
    温度under reflux
  3. 3
    温度by heating
  4. 4
    その他The solvent was removed under reduced pressure, and water and ethyl acetate
  5. 5
    workup.ADDITIONwere added
  6. 6
    その他The organic layer was separated
  7. 7
    抽出the aqueous layer was extracted with ethyl acetate
  8. 8
    洗浄the resultant solution was washed with an aqueous saturated sodium chloride solution
  9. 9
    乾燥dried over anhydrous magnesium sulfate
  10. 10
    その他the solvent was removed under reduced pressure

実験手順

To 30 mL of a xylene solution containing 2.3 g of methyl 3-oxo-3-(1,3-thiazol-2-yl)propionate, 1.4 mL of m-anisidine was added. The reaction mixture was stirred for 6 hours under reflux by heating. The solvent was removed under reduced pressure, and water and ethyl acetate were added thereto. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layer and the extract were combined, the resultant solution was washed with an aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure to obtain 3.3 g of a brown oily substance, N-(3-methoxyphenyl)-3-oxo-3-(1,3-thiazol-2-yl)propaneamide.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08524738B2uspto-grants-2013_09