تفاعل #2293216

ord-371e6b7fc1914a2ea2da9da7209baf22

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwith reflux under nitrogen atmosphere
  2. 2
    استخلاصthe mixture was extracted with ethyl acetate
  3. 3
    غسيلThe organic layer was washed successively with water and saturated brine
  4. 4
    تجفيفdried over anhydrous sodium sulfate
  5. 5
    تركيزconcentrated under reduced pressure
  6. 6
    أخرىThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

الإجراء التجريبي

A solution of 4-methoxy-1-phenyl-1H-pyrazolo[4,3-c]pyridin-3-yl trifluoromethanesulfonate (100 mg), 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzenesulfonamide (83 mg), tetrakis(triphenylphosphine)palladium(0) (31.0 mg) and 2M aqueous sodium carbonate solution (1.0 mL) in DME (10 mL) was heated overnight with reflux under nitrogen atmosphere. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The organic layer was washed successively with water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (101 mg).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09371320B2uspto-grants-2016_06