تفاعل #67989

ord-550d0306c7964def8c9e5963eb868381

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    درجة الحرارةunder reflux
  3. 3
    درجة الحرارةby heating
  4. 4
    أخرىThe solvent was removed under reduced pressure, and water and ethyl acetate
  5. 5
    workup.ADDITIONwere added
  6. 6
    أخرىThe organic layer was separated
  7. 7
    استخلاصthe aqueous layer was extracted with ethyl acetate
  8. 8
    غسيلthe resultant solution was washed with an aqueous saturated sodium chloride solution
  9. 9
    تجفيفdried over anhydrous magnesium sulfate
  10. 10
    أخرىthe solvent was removed under reduced pressure

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08524738B2uspto-grants-2013_09