HRID44436

反应详情

EQUATION

反应方程式

HRID 44436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. customAfter 5 minutes the solvents were removed by vacuum
  2. temperaturerefluxed for 5 hrs
  3. customThe reaction was quenched by the addition of an aqueous solution of 10% K2CO3 and 5% NaHSO3 (15 ml)
  4. extractionAfter extraction with dichloromethane
  5. dry with materialdrying the combined organic layers over MgSO4 the solvents
  6. customwere evaporated under reduced pressure
  7. customThe resulting crude product was purified by silica gel chromatography with (1:10) EtOAc