Reaktion #547155

ord-82e004982b844b9398cadb1d9ff86302

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstige7-(4-Diethylamino-butylamino)-3-(2,6-difluoro-3,5-dimethoxy-phenyl)-1-ethyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one was prepared
  2. 2
    SonstigeThe crude product was purified

Vorschrift

7-(4-Diethylamino-butylamino)-3-(2,6-difluoro-3,5-dimethoxy-phenyl)-1-ethyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one was prepared as described in Example 3 using 0.46 g (1.11 mmol) of 3-(2,6-difluoro-3,5-dimethoxy-phenyl)-1-ethyl-7-methylsulfinyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one and 0.32 g (2.22 mmol) of 4-diethylamino-butylamine. The crude product was purified using a gradient of 9:1 ethyl acetate/methanol to 9:0.25:0.25 to 9:0.5:0.25 ethyl acetate/methanol/triethylamine to give 0.4833 g (83%) of the title compound: mp 140° C.–141° C. MS (APCI) (m+1)/z 493.2.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07196090B2uspto-grants-2007_03