تفاعل #1605825

ord-8f28a22d5869481eb977534dd657f48a

الكواشف

لا شيء

المذيبات

ظروف التفاعل

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

المعالجة

  1. 1
    أخرىpurified water (10 mL)
  2. 2
    ترشيحThe reaction solution was filtered through celite, alumina, and Florisil
  3. 3
    استخلاصwas extracted with ethyl acetate
  4. 4
    غسيلThe organic layer was washed with a saturated aqueous solution of sodium chloride
  5. 5
    تجفيفdried over anhydrous magnesium sulfate
  6. 6
    تركيزconcentrated under reduced pressure

الإجراء التجريبي

4-Bromo-3-nitrobenzoic acid (1.0 g, 2.5 mmol) was dissolved in 1,4-dioxane (30 mL), and, thereto were added phenyl boric acid (610 mg, 5.0 mmol), cesium carbonate (6.5 g, 20.0 mmol), 1,1-[bis(diphenylphosphino)ferrocene]dichloropalladium(II) dichloromethane complex (204 mg, 0.10 mmol), and purified water (10 mL). The reaction mixture was stirred under a nitrogen flow at 80° C. overnight. The reaction solution was filtered through celite, alumina, and Florisil, and, thereafter, was extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 3-nitro-4-phenylbenzoic acid as a crude material.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09072734B2uspto-grants-2015_07