반응 #3548

ord-a307a99b72164a51b19fd145458a144d

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타above followed by purification on flash silica gel chromatography
  2. 2
    세척eluting sequentially with 100:0, 9:1, 4:1, and 7:3 ethyl acetate
  3. 3
    기타methanol gave an oil that
  4. 4
    기타was crystallized from ethyl acetate

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05733913uspto-grants-1998_03