反应详情

温度

25 °C

To a suspension of 2.9 g of potassium t-butoxide in 60 ml of DMF under a N2 atmosphere was added portionwise 7 g of the product of Example 1 while maintaining the reaction temperature at 25°-30° C. with an ice-water bath. After stirring at 25° C. for 1 hour, 7 g of methyl iodide was added dropwise to cause an exotherm to 37° C. The suspension was heated at 40°-60° C. for 5 hours, then cooled to 25° and poured onto excess ice-water to yield a precipitate. The suspension was filtered, and the isolated solid was dissolved in tetrahydrofuran and dried over MgSO4. The isolated solid was passed through a silica gel column with methylene chloride and, after evaporation of the first eluant, 5 g of the subject compound was obtained; m.p. 137°-140° C.

1. temperaturewhile maintaining the reaction temperature at 25°-30° C. with an ice-water bath
2. customto 37° C
3. temperatureThe suspension was heated at 40°-60° C. for 5 hours
4. temperaturecooled to 25°
5. customto yield a precipitate
6. filtrationThe suspension was filtered
7. dissolutionthe isolated solid was dissolved in tetrahydrofuran
8. dry with materialdried over MgSO4
9. customafter evaporation of the first eluant