反応 #3536

ord-62852d9a12b3459797e4f780f0a64cab

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.DISSOLUTIONwas dissolved
  2. 2
    ろ過filtered
  3. 3
    温度frozen

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05733913uspto-grants-1998_03