Reaktion #473852

ord-1441483351074a40bdf9209f95e30903

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeHCl was bubbled into the solution upon saturation
  2. 2
    workup.ADDITIONwas added
  3. 3
    Sonstigethe acetonitrile removed under vacuum
  4. 4
    Filtrationthe precipitate was filtered off
  5. 5
    Sonstigedried

Vorschrift

2-[(4-(imidazol-1-yl)-phenyl]-3-benzyloxy-6-amino-4H-1-benzopyran-4-one (3 g; 6.22 mmol) was suspended in acetonitrile (50 mL) and cooled at 0° C. HCl was bubbled into the solution upon saturation. The reaction was then stirred for 4 hours at r.t., upon completion, H2O (20 mL) was added and the acetonitrile removed under vacuum. The solution was then brought to pH=9 with NaOH 2N, the precipitate was filtered off and dried to give the titled compound as a bright yellow solid. Yield: 73%. TLC: (9/1 Chloroform/Methanol) Rf: 0.6.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08372866B2uspto-grants-2013_02