Reaktion #1939291

ord-d8b962ed65ce4c58b9d3e1fe6ca81920

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction was cooled
  2. 2
    Sonstigethe volatiles were removed under vacuum
  3. 3
    SonstigeThe crude residue was purified by silica gel chromatography
  4. 4
    SonstigeThe product factions were collected
  5. 5
    Sonstigethe solvent removed under vacuum

Vorschrift

To 1-chloro-6-fluoro-4-methoxyisoquinoline (200 mg, 0.945 mmol) was added dimethylamine 2 M in THF (2 ml, 4.00 mmol) and the solution was heated to 100° C. in a sealed tube for 16 h. The reaction was cooled and the volatiles were removed under vacuum. The crude residue was purified by silica gel chromatography using DCM as eluent. The product factions were collected and the solvent removed under vacuum to give 1-chloro-4-methoxy-N,N-dimethylisoquinolin-6-amine (150 mg, 70% yield). MS m/z 237.1 (M++1).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08957203B2uspto-grants-2015_02