HRID570691

反应详情

EQUATION

反应方程式

HRID 570691 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

7-Methoxy-2-(methylsulfanyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidin-4(3H)-one (1.55 g) and pyridine hydrochloride (3.1 g) were added to N,N-dimethylformamide (20 ml), and the mixture was stirred at 120° C. for 2 hr, and allowed to be cooled. The reaction mixture was poured into 0.5M hydrochloric acid (22 ml), and the white precipitate was collected by filtration, washed with water, and dissolved in tetrahydrofuran (30 ml). The solution was diluted with ethyl acetate (60 ml), dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was washed with ethyl acetate to give the title compound (1.33 g) as a white solid.

WORKUP

后处理

  1. temperatureto be cooled
  2. filtrationthe white precipitate was collected by filtration
  3. washwashed with water
  4. dissolutiondissolved in tetrahydrofuran (30 ml)
  5. additionThe solution was diluted with ethyl acetate (60 ml)
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. washThe obtained residue was washed with ethyl acetate