反応 #3546

ord-3b18944e08c244489c0c882a36845a09

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮concentrated in vacuo
  2. 2
    乾燥The organic phase was dried over magnesium sulfate
  3. 3
    濃縮concentrated to a glass that
  4. 4
    その他was crystallized from acetonitrile

実験手順

To a suspension of 210 mg (1 mmol) of 7-amino-6-(2,6-dichlorophenyl)-2-[3-(diethylamino) propylamino]-pyrido[2,3-d]pyrimidine from Example 20 in 0.8 mL of DMF was added 0.8 mL of DMF dimethyl acetal. The mixture was stirred at room temperature for 5.5 hours, then concentrated in vacuo. The residual oil was distributed between dichloromethane and water. The organic phase was dried over magnesium sulfate, then concentrated to a glass that was crystallized from acetonitrile to give 160 mg (68%) of N'-[6-(2,6-dichlorophenyl)-2-{3-(diethylamino) propylamino}-pyrido[2,3-d]pyrimidin-7-yl]-N, N-dimethylformamidine, mp 100°-104° C.

出典

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