反应详情

To a cold (−10° C.) solution of EXAMPLE 454C (1.18 g) and toluenesulfonylmethyl isocyanide (2.268 g) in dimethoxyethane (3 mL) and absolute ethanol (0.1 mL) was added portionwise potassium tert-butoxide (2.235 g). The reaction mixture was continued to stir maintaining the temperature below 5° C. for 30 minutes, warmed to room temperature, heated at 35° C. for 30 minutes and then at room temperature for 2 hours. The reaction mixture was concentrated and the residue was dissolved in water-brine, extracted with dichloromethane. The dichloromethane layer was purified by flash chromatography, eluted with 5% ethyl acetate in dichloromethane to provide the title compound.

1. temperaturemaintaining the temperature below 5° C. for 30 minutes
2. temperatureheated at 35° C. for 30 minutes
3. concentrationThe reaction mixture was concentrated
4. dissolutionthe residue was dissolved in water-brine
5. extractionextracted with dichloromethane
6. customThe dichloromethane layer was purified by flash chromatography
7. washeluted with 5% ethyl acetate in dichloromethane