反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Tert-butyl piperazine-1-carboxylate (300 mg, 1.611 mmol) and 2-bromo-5-chloropyridine (465 mg, 2.416 mmol) were dissolved in acetonitrile (3 ml), followed by addition of triethylamine (0.45 ml, 3.222 mmol), and then the resulting liquid was subjected to microwave irradiation at 150° C. for 2 hours. The resulting reaction liquid was concentrated under reduced pressure, followed by addition of a saturated aqueous ammonium chloride solution (10 ml), and extracted with MC (15 ml×2). The organic layer was dried over anhydrous sodium sulfate, followed by filtration and concentration, and then the residue thus obtained was subjected to MPLC (20% EtOAc/Hexanes), to obtain 177 mg of colorless oil (37%).
WORKUP
后处理
- customirradiation at 150° C. for 2 hours
- customThe resulting reaction liquid
- concentrationwas concentrated under reduced pressure
- additionfollowed by addition of a saturated aqueous ammonium chloride solution (10 ml)
- extractionextracted with MC (15 ml×2)
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- filtrationfollowed by filtration and concentration
- customthe residue thus obtained