HRID3452

反应详情

EQUATION

反应方程式

HRID 3452 的结构方程式

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. customabove followed by purification on flash silica gel chromatography
  2. washeluting sequentially with 100:0, 9:1, 4:1, and 7:3 ethyl acetate
  3. custommethanol gave an oil that
  4. customwas crystallized from ethyl acetate