تفاعل #794390

ord-4d9aa523a6c74f02b1a4655c30ea52ba

الكواشف

لا شيء

المذيبات

ظروف التفاعل

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

المعالجة

  1. 1
    أخرىprepared in Example 3
  2. 2
    درجة الحرارةThe reaction mixture was cooled to room temperature
  3. 3
    غسيلthe mesh catalyst precursor was washed with ethanol
  4. 4
    workup.DISTILLATIONThe solvent was distilled away from the reaction mixture under reduced pressure
  5. 5
    أخرىThe residue was purified by column chromatography on silica gel (n-hexane)

الإجراء التجريبي

To a solution of iodobenzene (102 mg), 4-chlorophenylboronic acid (117 mg), and potassium carbonate (138 mg) in ethanol (3 ml) was added the mesh catalyst precursor (12 mm by 14 mm) prepared in Example 3 and heated for 12 hours at 80° C. The reaction mixture was cooled to room temperature, and the mesh catalyst precursor was washed with ethanol and taken off from the mixture. The solvent was distilled away from the reaction mixture under reduced pressure. The residue was purified by column chromatography on silica gel (n-hexane) to give an intended product, 4-chlorobiphenyl quantitatively. The mesh catalyst precursor taken off from the mixture was again used in the same reaction to again give the intended product, 4-chlorobiphenyl quantitatively. The mesh catalyst precursor could be recycled at least thirty times.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09175004B2uspto-grants-2015_11