Reaktion #1277418

ord-6e6b71dab2514ea1be14abefbfe8b265

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    Filtrationthe solid is filtered off with suction
  3. 3
    Waschenwashed three times with 100 ml of ethanol each time
  4. 4
    Waschenwashed twice
  5. 5
    Filtrationeach time filtered off with suction
  6. 6
    WaschenThe solid is finally washed once with boiling ethanol

Vorschrift

Procedure analogous to Example 3a. Instead of 149.0 ml (1.2 mol) of 1,2-dibromobenzene and 98.0 g (308 mmol) of 9,10-anthracenediboronic acid ethylene glycol ester, 12.1 ml (100 mmol) of dibromobenzene and 68.0 g (306 mmol) of 9-anthraceneboronic acid are used. After cooling, the solid is filtered off with suction, washed three times with 100 ml of ethanol each time and then washed twice by stirring with 1000 ml of refluxing acetic acid each time (1 h) and each time filtered off with suction after cooling to 90° C. The mother liquor is discarded in each case. The solid is finally washed once with boiling ethanol. Yield: 33.0 g (76 mmol), 76.6% of theory; purity: 98% according to 1H-NMR.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08674141B2uspto-grants-2014_03