反应详情

温度

60 °C

To a solution of 6-bromo-1-methyl-2,2-dioxo-pyrido[3,2-c]thiazin-4-one (456 mg, 1.56 mmol) in DMF (3 ml) was added K2CO3 (2.16 g, 15.6 mmol) followed by Mel (0.29 ml, 4.7 mmol) at ambient temperature. The suspension was heated to 60° C. for 1.5 h then cooled to ambient temperature, filtered, washed with ethyl acetate and concentrated under reduced pressure. Purification by flash chromatography eluting with ethyl acetate/heptane, gradient, afforded 6-bromo-1,3,3-trimethyl-2,2-dioxo-pyrido[3,2-c]thiazin-4-one.

1. customfollowed by Mel (0.29 ml, 4.7 mmol) at ambient temperature
2. temperaturethen cooled to ambient temperature
3. filtrationfiltered
4. washwashed with ethyl acetate
5. concentrationconcentrated under reduced pressure
6. customPurification by flash chromatography
7. washeluting with ethyl acetate/heptane, gradient