تفاعل #68013

ord-107b4fe204144bcb9cc1d7668ea6b5b5

ظروف التفاعل

درجة الحرارة
40°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITat room temperature for 5 days
  2. 2
    أخرىThe solvent was removed under reduced pressure
  3. 3
    workup.ADDITIONthe reaction mixture was added with ethyl acetate
  4. 4
    أخرىThe organic layer was separated
  5. 5
    استخلاصthe aqueous layer was extracted with ethyl acetate
  6. 6
    غسيلthe resultant solution was washed with an aqueous saturated sodium chloride solution
  7. 7
    تجفيفdried over anhydrous magnesium sulfate
  8. 8
    أخرىthe solvent was removed under reduced pressure

الإجراء التجريبي

To 0.17 g of 1-(1,3-dioxolan-2-ylmethyl)-8-methylquinolin-2(1H)-one, 2 mL of a 90% aqueous trifluoroacetic acid solution was added, and the mixture was stirred at room temperature for 4 days, at 40° C. for 3 days, and at room temperature for 5 days. The solvent was removed under reduced pressure, and the reaction mixture was added with ethyl acetate and an aqueous saturated sodium hydrogen carbonate solution. 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 0.14 g of a brown oily substance, (8-methyl-2-oxoquinolin-1(2H)-yl)acetaldehyde.

المصدر

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