HRID69972

反应详情

EQUATION

反应方程式

HRID 69972 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureUpon cooling to room temperature
  2. extractionthe mixture was extracted with EtOAc
  3. dry with materialdried with Na2SO4
  4. concentrationconcentrated
  5. customThe crude material was purified via SiO2 column chromatography
  6. washeluting with DCM/MeOH (2%)