HRID522159

反应详情

EQUATION

反应方程式

HRID 522159 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 2,3-dichloro-6-methylpyridine (2 g, 12.3 mmol) in carbon tetrachloride (40 mL) was added NBS (2.64 g, 14.8 mmol) followed by AIBN (40 mg, 0.24 mmol). The reaction heated to 80° C. under nitrogen for 3.5 hours. The reaction was cooled and concentrated in vacuo. The residue was sonicated in heptanes and filtered. The filtrate was eluted through a pad of silica using 10% TBME in heptanes to afford the title compound (2.90 g). The crude material was taken on directly to the next step.

WORKUP

后处理

  1. temperatureThe reaction was cooled
  2. concentrationconcentrated in vacuo
  3. customThe residue was sonicated in heptanes
  4. filtrationfiltered
  5. washThe filtrate was eluted through a pad of silica using 10% TBME in heptanes