تفاعل #6994

ord-46b34f726ee24169b4da1dd46149cf32

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
105°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONA flame-dried flask containing N2 inlet and magnetic stirrer
  2. 2
    درجة الحرارةcooled to room temperature
  3. 3
    أخرىpartitioned between water and EtOAc
  4. 4
    غسيلthe combined organic layers were successively washed with 2N NaOH, water and saturated aqueous NaCl
  5. 5
    تجفيفAfter drying with MgSO4
  6. 6
    أخرىthe solvent was removed

الإجراء التجريبي

A flame-dried flask containing N2 inlet and magnetic stirrer was charged with 2.9 g (18 mmol) of 3,4-dichlorophenol, 6.2 g (45 mmol) of potassium carbonate and 50 mL of anhydrous DMF. With stirring, 2.08 g (15 mmol) of 2,5-difluorobenzonitrile (Aldrich Chem. Co.) was added and the mixture was heated overnight at 105° C., cooled to room temperature and partitioned between water and EtOAc. The aqueous layer was reextracted with EtOAc and the combined organic layers were successively washed with 2N NaOH, water and saturated aqueous NaCl. After drying with MgSO4, the solvent was removed to give the title product as a light brown oil which slowly solidified, 3.5 g.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07084165B2uspto-grants-2006_08