Reaktion #2323812

ord-1528c0fd74204ed9af8dc01d5c4f617b

Lösungsmittel

Reaktionsbedingungen

Temperatur
115°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturUpon cooling to room temperature
  2. 2
    Sonstigethe product precipitated out
  3. 3
    FiltrationThe precipitate is then filtered off
  4. 4
    Waschenwashed with water
  5. 5
    Sonstigedried

Vorschrift

To a suspension of crude 6-Bromo-4-methoxymethylene-4H-isoquinoline-1,3-dione (423 mg, 1.5 mmol) in N,N-dimethylformamide (3 mL) is added 4-(4-Methyl-piperazin-1-yl)-phenylamine (290 mg, 1.5 mmol). The reaction mixture is shaken at 115° C. for 1.5 hours. Upon cooling to room temperature and addition of 2 mL of water, the product precipitated out. The precipitate is then filtered off, washed with water, and dried to yield 0.5 g of crude 6-bromo-4-{[4-(4-methyl-piperazin-1-yl)-phenylamino]-methylene}-4H-isoquinoline-1,3-dione, which is used as such for the next reaction.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07713994B2uspto-grants-2010_05