HRID42186

反应详情

EQUATION

反应方程式

HRID 42186 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Solid Na2CO3 (50 mg, 0.47 mmol, 1.5 eq) is added to a solution of 6-chloronicotinonitrile (50 mg, 0.36 mmol, 1.2 eq), 1-benzyl-4-((R)-3-methyl-piperazin-1-yl)-phthalazine (100 mg, 0.31 mmol, 1.0 eq) in DMF (1 mL) and dioxane (2 mL) in a microwave vial. The vial is sealed and irradiated in the microwave at 180° C. (high absorption setting) for 30 minutes. The reaction mixture is concentrated, dichloromethane is added and is washed with water then brine. The organic fraction is dried over sodium sulfate, and is evaporated under reduced pressure, then purified by flash chromatography (50%-90% EtOAc/Hexane) to afford the title compound as a white solid (55 mg, 42% yield).

WORKUP

后处理

  1. customThe vial is sealed
  2. customirradiated in the microwave at 180° C. (high absorption setting) for 30 minutes
  3. concentrationThe reaction mixture is concentrated
  4. additiondichloromethane is added
  5. washis washed with water
  6. dry with materialThe organic fraction is dried over sodium sulfate
  7. customis evaporated under reduced pressure
  8. custompurified by flash chromatography (50%-90% EtOAc/Hexane)