反応 #3282

ord-a8f31c3f69e44f889459e4fbf80bb158

反応条件

温度
110°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

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