HRID447079

反应详情

EQUATION

反应方程式

HRID 447079 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

To a solution of 3-benzyl-4,5-dimethyl-6-(1,2,3,6-tetrahydropyridin-4-yl)pyridazine (70 mg, 0.175 mmol) in 2 mL dioxane is added 2-chloro-5-(trifluoromethyl)pyridine (64 mg, 0.35 mmol) and TEA (0.122 mL, 0.88 mmol) in a microwave tube. The reaction mixture is heated at 160° C. for 40 min in a microwave reactor. The mixture is concentrated to afford a brown oil and purified by prep HPLC, eluting with 10%-100% acetonitrile:water (both mobile phases modified by 3% n-PrOH). Fractions containing the desired product are combined and freeze-dried to afford a white solid (33 mg, 42%).

WORKUP

后处理

  1. concentrationThe mixture is concentrated
  2. customto afford a brown oil
  3. custompurified by prep HPLC
  4. washeluting with 10%-100% acetonitrile
  5. additionFractions containing the desired product
  6. customfreeze-dried