反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
5 g (22.6 mM) of 5-hydroxy-2-iodopyridine and 6.42 ml (30.09 mM) of triisopropylsilyl chloride in 35 ml of acetonitrile are stirred at room temperature for 10 minutes. After the addition of 4.62 g (67.87 mM) of imidazole, stirring is maintained for 4 h 20 min at room temperature. The acetonitrile is evaporated off and the reaction mixture is taken up with three 150 ml portions of pentane. The combined organic phases are washed with saturated sodium chloride solution, dried over magnesium sulfate and concentrated under reduced pressure. The evaporation residue is passed through a silica plug using petroleum ether as the eluent to give the desired product in the form of a light yellow oil with a yield of 98%.
WORKUP
后处理
- customThe acetonitrile is evaporated off
- washThe combined organic phases are washed with saturated sodium chloride solution
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under reduced pressure