HRID59153

反应详情

EQUATION

反应方程式

HRID 59153 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 2-chloro-N-methyl-6-((2,2,2-trifluoroethoxy)methyl)pyrimidin-4-amine (50 mg, 0.20 mmol), 3-methoxy-4-(6-methylpyridazin-4-yl)aniline (42 mg, 0.20 mmol), cesium rbonate (127 mg, 0.39 mmol), palladium (II) acetate (7 mg, 0.03 mmol) and 2-(dicyclohexylphosphino)-biphenyl (10 mg, 0.03 mmol) in dioxane (2 mL) was heated under argon at 120° C. for 90 minutes in a microwave reactor. 2-Chloro-N-methyl-6-((2,2,2-trifluoroethoxy)methyl)pyrimidin-4-amine (72 mg, 0.28 mmol, 1.4 eq), palladium(II) acetate (7 mg) and 2-(dicyclohexylphosphino)biphenyl (10 mg) was added and the mixture was heated at 120° C. for 90 minutes in a microwave reactor. The mixture was filtered through a short silica gel plug which was washed with 10% solution of methanol in ethyl acetate (75 mL). The eluate was concentrated in vacuum and the residue was purified by preparative to give the title compound as a solid, 22 mg (26%).

WORKUP

后处理

  1. temperaturethe mixture was heated at 120° C. for 90 minutes in a microwave reactor
  2. filtrationThe mixture was filtered through a short silica gel plug which
  3. washwas washed with 10% solution of methanol in ethyl acetate (75 mL)
  4. concentrationThe eluate was concentrated in vacuum
  5. customthe residue was purified by preparative