تفاعل #1772998

ord-59b3ec64bbed42768f20b6c96420d10d

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصthe mixture was extracted with ethyl acetate
  2. 2
    غسيلThe organic layer was washed with water and saturated brine
  3. 3
    تجفيفdried over anhydrous magnesium sulfate
  4. 4
    أخرىThe solvent was evaporated under reduced pressure
  5. 5
    أخرىthe residue was purified by silica gel column chromatography (chloroform/methanol=10/1)

الإجراء التجريبي

Ethyl 2-[4-(2-oxothiolan-3-ylidenemethyl)phenyl]propionate (124 mg) obtained in Example 34 was dissolved in 1,4-dioxane (4.0 ml), and then to the solution was added 30% aqueous sulfuric acid (4.0 ml). The reaction mixture was stirred at room temperature for 4 days, then added to water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (chloroform/methanol=10/1) to give the title compound (65 mg, 58%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08148421B2uspto-grants-2012_04