HRID44436
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
PROCEDURE
实验过程
To the 2-chloro-3-phenylquinoxaline (4.15 mmol) in dry THF (10 ml) was added a solution of 2 M HCl in ether (4 ml). After 5 minutes the solvents were removed by vacuum. Dry sodium iodide (41.5 mmol) and acetonitrile (30 ml) were added to the hydrochloride salt and refluxed for 5 hrs. The reaction was quenched by the addition of an aqueous solution of 10% K2CO3 and 5% NaHSO3 (15 ml). After extraction with dichloromethane, and drying the combined organic layers over MgSO4 the solvents were evaporated under reduced pressure. The resulting crude product was purified by silica gel chromatography with (1:10) EtOAc:hexane, to give 95% yield of the desired product.
WORKUP
后处理
- customAfter 5 minutes the solvents were removed by vacuum
- temperaturerefluxed for 5 hrs
- customThe reaction was quenched by the addition of an aqueous solution of 10% K2CO3 and 5% NaHSO3 (15 ml)
- extractionAfter extraction with dichloromethane
- dry with materialdrying the combined organic layers over MgSO4 the solvents
- customwere evaporated under reduced pressure
- customThe resulting crude product was purified by silica gel chromatography with (1:10) EtOAc