Reaktion #6908

ord-d57d16896f9f4187ad5a58a2a543f654

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationthe reaction was filtered through CELITE diatomaceous earth
  2. 2
    Waschenwashed copiously with methanol
  3. 3
    SonstigeThe volatiles were removed under vacuum
  4. 4
    Sonstigethe crude residue was triturated with ether
  5. 5
    SonstigeThe solids were collected on a fritted funnel
  6. 6
    Sonstigedried under vacuum

Vorschrift

3,4-Dihydroquinolin-2(1H)-one (7.5 g; 51 mmol) and silver (I) sulfate (17.5 g; 56.1 mmol) were suspended in ethanol (250 mL). A solution of iodine in ethanol (250 mL) was added slowly to the reaction over 1 hour. After 6 hours, the reaction was filtered through CELITE diatomaceous earth and washed copiously with methanol. The volatiles were removed under vacuum and the crude residue was triturated with ether. The solids were collected on a fritted funnel and dried under vacuum. This provided the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07084156B2uspto-grants-2006_08