تفاعل #365747

ord-08186b392d05445ba3a70fe0619d71c2

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwith reflux under nitrogen atmosphere
  2. 2
    استخلاصthe solution was extracted with ethyl acetate
  3. 3
    غسيلThe extract was washed with water
  4. 4
    تجفيفdried (MgSO4)
  5. 5
    تركيزconcentrated
  6. 6
    غسيلeluted with hexane-ethyl acetate (2:1)

الإجراء التجريبي

To a mixture of ethyl 4-bromobenzoate (2.29 g), 4-pyridyl borate (1.23 g), 1 M sodium hydrogen carbonate solution (30 ml) and 1,2-dimethoxyethane (40 ml) was added tetrakis(triphenylphosphine)palladium (0.3 g) and the mixture was stirred for 3 hours with reflux under nitrogen atmosphere. To the mixture was added water and the solution was extracted with ethyl acetate. The extract was washed with water, dried (MgSO4) and concentrated. The residue was subjected to silica gel chromatography, and eluted with hexane-ethyl acetate (2:1) to give the title compound as crystals (1.15 g, 50.7%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06359134B1uspto-grants-2002_03