反応 #3548

ord-a307a99b72164a51b19fd145458a144d

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他above followed by purification on flash silica gel chromatography
  2. 2
    洗浄eluting sequentially with 100:0, 9:1, 4:1, and 7:3 ethyl acetate
  3. 3
    その他methanol gave an oil that
  4. 4
    その他was crystallized from ethyl acetate

実験手順

2,7-Diamino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidine from Example 1 was reacted with DMF dimethyl acetal for 23 hours as described in Example 78. Workup as described above followed by purification on flash silica gel chromatography eluting sequentially with 100:0, 9:1, 4:1, and 7:3 ethyl acetate:methanol gave an oil that was crystallized from ethyl acetate to afford N'-[6-(2,6-dichlorophenyl)-7-[(dimethylamino)-methyleneamino]-pyrido[2,3-d]pyrimidin-2-yl]-N,N-dimethylformamidine, mp 269°-272° C.

出典

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