HRID69972
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
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
To a solution of 4,6-dichloropyridin-2-amine (1.0 equiv.) in THF (0.1M) was added Pd(dppf)Cl2-DCM (0.1M), K2CO3 (3.0 equiv.), and Et2Zn (1.2 equiv.). The reaction was heated to 70° C. for 18 hrs. Upon cooling to room temperature, NH4Cl(sat.) was added, the mixture was extracted with EtOAc, dried with Na2SO4, and concentrated. The crude material was purified via SiO2 column chromatography eluting with DCM/MeOH (2%) to yield 4-chloro-6-ethylpyridin-2-amine in 33% yield. LCMS (m/z): 157.1 (MH+).
WORKUP
后处理
- temperatureUpon cooling to room temperature
- extractionthe mixture was extracted with EtOAc
- dry with materialdried with Na2SO4
- concentrationconcentrated
- customThe crude material was purified via SiO2 column chromatography
- washeluting with DCM/MeOH (2%)