تفاعل #617365

ord-67f7b26c2ed24c3ebedb3ecc71d7e8b7

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىto react at 90° C. for 7 hours
  2. 2
    درجة الحرارةAfter cooling
  3. 3
    ترشيحthe reaction solution was filtered
  4. 4
    أخرىsolids obtained
  5. 5
    غسيلwere washed with methanol and clean water
  6. 6
    أخرىFurther, the solids were purified by silica gel chromatography (heated toluene)

الإجراء التجريبي

Under an argon atmosphere, 15.0 g of 1,6-dibromopyrene, 13.2 g of phenylboronic acid, 1.9 g of tetrakis(triphenylphosphine)palladium (0) [Pd(PPh3)4], 27.8 g of sodium carbonate (130 mL of clean water), toluene and tetrahydrofuran were placed into a flask, and the resulting mixture was allowed to react at 90° C. for 7 hours. After cooling, the reaction solution was filtered, and solids obtained were washed with methanol and clean water. Further, the solids were purified by silica gel chromatography (heated toluene). The resulting crude product which was obtained by a concentration was re-crystallized from toluene, followed by drying under a reduced pressure, whereby white solids of 1,6-diphenylpyrene (11.8 g) were obtained.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09353027B2uspto-grants-2016_05