HRID1254063
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
- 0 °C
PROCEDURE
实验过程
1-(6-Bromopyridin-3-yl)ethanone was dissolved in 50 mL of chloroform and cooled to 0° C., to which was added catalytic amount of AlCl3 and 2.65 mL of bromine in 25 mL of chloroform. The addition of bromine lasted 1 h to keep the reaction solution at 0° C. After stirring at 0° C. overnight, the mixture was diluted with dichloromethane, washed with aqueous sodium bicarbonate, water, and brine. The organic layer was dried (MgSO4), filtered, and concentrated to afford 2-bromo-1-(6-bromopyridin-3-yl)ethanone which was used in the next step with out further purification. LCMS: [M+1]+=279.
WORKUP
后处理
- customat 0° C
- washwashed with aqueous sodium bicarbonate, water, and brine
- dry with materialThe organic layer was dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated