تفاعل #43326

ord-2d12e7bdf6a04c519d5deb44ecdd7cfa

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلwashed with saturated aqueous sodium bicarbonate solution and saturated brine
  2. 2
    تجفيفdried over anhydrous potassium carbonate
  3. 3
    تركيزConcentrating the solvent under reduced pressure
  4. 4
    أخرىthe resulting residue was crystallized
  5. 5
    workup.ADDITIONfrom mixed solvent of ethyl acetate and hexane

الإجراء التجريبي

A catalytic amount of pyridinium p-toluenesulfonate and 3,4-dihydro-2H-pyrane (0.8 mL, 8.89 mmols) were added to a dichloromethane (30 mL) solution of 4,5-dibromo-2-(4-hydroxyphenyl)-2H-pyridazin-3-one (1.03 g, 2.98 mmols), and stirred at room temperature for 2 hours, washed with saturated aqueous sodium bicarbonate solution and saturated brine, and dried over anhydrous potassium carbonate. Concentrating the solvent under reduced pressure, the resulting residue was crystallized from mixed solvent of ethyl acetate and hexane to provide the title compound (1.1 g, 86%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07732456B2uspto-grants-2010_06