反应详情

5.5 g (30 mmol) of the chloro compound (Example 1, Step B) and 4.0 g (30 mmol) of N-chlorosuccinimide were dissolved in 150 ml chloroform, stirred for 4 h at room temperature, and finally heated for some minutes on a steam bath. The mixture was poured on to ice water, the aqueous layer extracted with dichloromethane, the combined organic layers washed twice with saturated sodium carbonate solution, dried over sodium sulfate, and evaporated in in vacuo. The title compound was obtained as an oil after chromatography on silica gel with dichloromethane.

1. temperaturefinally heated for some minutes on a steam bath
2. extractionthe aqueous layer extracted with dichloromethane
3. washthe combined organic layers washed twice with saturated sodium carbonate solution
4. dry with materialdried over sodium sulfate
5. customevaporated in in vacuo