Reaktion #1244

ord-92bc8cb4ed55424491eb833aaed1c16a

Reaktionsgleichung

Fc1ccc(-c2onc3ccccc23)cc1
( 16 )
Fc1ccc(-c2onc3ccccc23)cc1
3-(4-fluorophenyl)-2,1-benzisoxazole
Nc1ccccc1C(=O)c1ccc(F)cc1
2-amino-4'-fluorobenzophenone

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe vigorously stirred suspension is flushed with hydrogen gas
  2. 2
    Sonstige8-10 hours
  3. 3
    SonstigeThe catalyst is removed by filtration through a bed of celite
  4. 4
    Sonstigethe solvent is removed under reduced pressure
  5. 5
    SonstigeThe product (16) is recrystallized from toluene

Vorschrift

To a suspension of (16) (42.6 g, 0.2 mol) in 750 ml of dry tetrahydrofuran (THF) and 20 ml of triethylamine is added 5% palladium on charcoal (6 g). The vigorously stirred suspension is flushed with hydrogen gas and stirred at room temperature under a hydrogen atmosphere until absorption of hydrogen ceases (approximately 90-90% of the molar amount; 8-10 hours). The catalyst is removed by filtration through a bed of celite, and the solvent is removed under reduced pressure. The product (16) is recrystallized from toluene.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05723573uspto-grants-1998_03