Reaktion #8809

ord-3ea103740d49442d947174854bfe2809

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated
  2. 2
    Temperaturat reflux for 72 h
  3. 3
    SonstigeThe solvent was removed under reduced pressure
  4. 4
    SonstigeThe gummy residue was triturated with isopropanol
  5. 5
    Filtrationthe resulting crystals filtered
  6. 6
    SonstigeRecrystallization from dichloromethane

Vorschrift

3-Chloro-6,7-dimethoxy-2H-benzo[1,2,4]thiadiazine-1,1-dioxide 1a (154 mg, 0.55 mmol) and 6,7-dimethoxy-1,2,3,4-tetrahydroisoquinoline 2a (wherein R1 and R4 are hydrogen, and R2 and R3 are methoxy) (138 mg, 0.6 mmol) were dissolved in 20 ml of methoxyethanol and heated at reflux for 72 h. The solvent was removed under reduced pressure. The gummy residue was triturated with isopropanol and the resulting crystals filtered. Recrystallization from dichloromethane afforded 120 mg of 3-(6,7-dimethoxy-3,4-dihydro-1H-isoquinolin-2-yl)-6,7-dimethoxy-2H-benzo[1,2,4]thiadiazine-1,1-dioxide 101, [M+H]+=434.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07091200B2uspto-grants-2006_08