Reaktion #79422

ord-238eb57abbf748bb8dc0e33ebc47f885

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe mixture was evaporated
  2. 2
    FiltrationThis was then filtered through celite
  3. 3
    Sonstigethe solvent evaporated
  4. 4
    SonstigeThe gummy residue was then triturated with hexane giving a beige solid
  5. 5
    SonstigeThis material was further purified by column chromatography

Vorschrift

(4-Benzyloxy-phenyl)-(6-chloro-pyrido[3,4-d]pyrimidin-4-yl)-amine (1.4 g) and 3-(1,3-dioxolan-2-yl)-phenyl-tributylstannane (3.08 g) [A. Lee and W-C. Dai, Tetrahedron (1997), 53(3), 859-868] in dioxan (30 ml) were reacted together as in Procedure B. The mixture was evaporated and the residue suspended in dichloromethane. This was then filtered through celite and the solvent evaporated. The gummy residue was then triturated with hexane giving a beige solid. This material was further purified by column chromatography, giving a brown foam (252 mg); m/z 477 (M+1)+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06713485B2uspto-grants-2004_03