反应 #3282

ord-a8f31c3f69e44f889459e4fbf80bb158

反应条件

温度
110°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    温度After 20 hours reflux
  3. 3
    其他the excess amine and dimethylformamide were evaporated
  4. 4
    其他the residue was triturated with water
  5. 5
    过滤filtered
  6. 6
    洗涤washed with water
  7. 7
    其他dried
  8. 8
    其他Recrystallization from ethyl acetate/petroleum ether
  9. 9
    其他gave pure product

实验过程

A mixture of 0.177 g (0.50 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 37, 10 mL of n-butylamine and 1.0 mL of dimethylformamide was heated with stirring to reflux (110° C. oil bath). After 1 hour, solution was complete. After 20 hours reflux, the excess amine and dimethylformamide were evaporated, and the residue was triturated with water, filtered, washed with water, and dried; wt 0.180 g. Recrystallization from ethyl acetate/petroleum ether gave pure product; wt 0.116 g; mp 184°-186° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05733914uspto-grants-1998_03