反应详情

Compound 8 (1.5 g) was dissolved in dichloromethane (10 mL). Potassium carbonate (980 mg) and the solution of bromoacetyl chloride (890 mg) in dichloromethane (5 mL) was added thereto at 0° C., followed by stirring for 1.5 hours. The reaction solution cooled with ice was poured into 1N hydrochloric acid, followed by extraction with dichloromethane. The organic layer was washed with an aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1) to obtain the title compound (1.7 g) having the following physical property values.

1. customat 0° C.
2. temperatureThe reaction solution cooled with ice
3. extractionfollowed by extraction with dichloromethane
4. washThe organic layer was washed with an aqueous saturated sodium chloride solution
5. dry with materialdried with anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=4:1)