تفاعل #1100089

ord-d37b9a12e8084b1fbfd2a2000a4239d7

المذيبات

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwere added to a 1-L three-necked flask
  2. 2
    أخرىequipped with a cooling pipe
  3. 3
    درجة الحرارةthe whole was refluxed
  4. 4
    workup.ADDITIONwas added
  5. 5
    ترشيحa crystal was filtered out
  6. 6
    غسيلwashed with 50 mL of water, 100 mL of ethanol, and 100 mL of toluene

الإجراء التجريبي

In a stream of argon, 20 g (55.6 mmol) of 1,6-dibromopyrene, 16.3 g (133 mmol) of phenyl boronic acid, 2.5 g (4 mol %) of tetrakistriphenylphosphine palladium, an aqueous solution containing 26.5 g (65 mmol) of sodium carbonate in 125 mL of water, and 250 mL of toluene were added to a 1-L three-necked flask equipped with a cooling pipe, and the whole was refluxed under heat at 100° C. for 8 hours. After the completion of the reaction, 50 mL of water was added and then a crystal was filtered out, washed with 50 mL of water, 100 mL of ethanol, and 100 mL of toluene. As a result, 15.3 g of 1,6-diphenylpyrene (a white powder) was obtained (99% yield).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07981523B2uspto-grants-2011_07