Reaktion #3536

ord-62852d9a12b3459797e4f780f0a64cab

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISSOLUTIONwas dissolved
  2. 2
    Filtrationfiltered
  3. 3
    Temperaturfrozen

Vorschrift

To a solution of 1-[6-(2,6-dichlorophenyl)-2-(4-diethylamino-butylamino)-pyrido[2,3-d]pyrimidin-7-yl]-3-ethyl-urea (3.253 g) from Example 55 in water (250 mL) was added one equivalent of 1N hydrochloric acid (6.44 mL). The solution was stirred at room temperature until the solid was dissolved, filtered, and frozen. Lyophilization gave 3.63 g the hydrochloric acid salt of 1-[6-(2,6-dichlorophenyl)-2-(4-diethylamino-butylamino)-pyrido[2,3-d]pyrimidin-7-yl]-3-ethyl-urea, ESMS (20/80 MeOH/CH3CN+1% AcOH): M+ +H=504; mp dec >50° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05733913uspto-grants-1998_03