تفاعل #8089

ord-91f9a9d242cc4d829d962d9a6373321d

المذيبات

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىto drop back to room temperature
  2. 2
    استخلاصThe mixture was then extracted with ethyl acetate
  3. 3
    غسيلThe extract was washed with brine
  4. 4
    تجفيفdried over anhydrous sodium sulfate
  5. 5
    workup.DISTILLATIONThe solvent was distilled off
  6. 6
    أخرىthe residue was reacted

الإجراء التجريبي

To a solution of 4-methoxycarbonyl-6-[4-(methylthio)-phenyl]-2H-pyridazin-3-one (8.00 g, 29.0 mmol) in N,N-dimethylformamide (80 mL) were added potassium carbonate (8.02 g, 58.0 mmol) and isobutyl bromide (4.76 g, 34.8 mmol), and the mixture was stirred at 80° C. for 2 hours. The temperature of the reaction mixture was allowed to drop back to room temperature, and a saturated aqueous solution of sodium hydrogencarbonate was added. The mixture was then extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was distilled off. Following the procedure of Example 1 (7), the residue was reacted to yield the title compound as a yellow solid [yield: 65.1% (2 steps)].

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07087606B2uspto-grants-2006_08