反应 #67989

ord-550d0306c7964def8c9e5963eb868381

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

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