反应详情

Potassium carbonate (11.4 mmole) was added to a solution of the product of Example 4 (5.7 mmole) in 50 ml xylene, heated to reflux, and the water formed removed with a Dean-Stark trap. After 1 hour the Dean-Stark trap was drained. The solution was cooled to room temperature and methyl p-toluenesulfonate (17.1 mmole) added. The solution was heated to 70° C. for 20 hours, and refluxed for one hour to remove the water formed. After the white solid was filtered and discarded, the filtrate was concentrated under vacuum to a solid, which was was recrystallized from hot hexane, to give the title compound (1.6 g), m.p. ca. 73°-74° C.

1. temperatureheated
2. temperatureto reflux
3. customremoved with a Dean-Stark trap
4. temperatureThe solution was heated to 70° C. for 20 hours
5. temperaturerefluxed for one hour
6. customto remove the water
7. customformed
8. filtrationAfter the white solid was filtered
9. concentrationthe filtrate was concentrated under vacuum to a solid, which
10. customwas was recrystallized from hot hexane