反应详情

Cyanogen bromide (2.9 g, 0.027 mol) was added to a mixture of the compound prepared in Step 1 above (6.1 g, 0.025) and KHCO3 (2.8 g, 0.028 mol) in dioxane/water (1:1, 50 mL) at room temperature. The mixture was refluxed for 1 hour, allowed to cool, filtered, washed with dioxane/water (1:1, 20 mL), then water (50 mL), and dried in vacuo. The solid was recrystallized from chloroform to yield 4.16 g, m.p. 147°-150° C.

1. temperatureThe mixture was refluxed for 1 hour
2. temperatureto cool
3. filtrationfiltered
4. washwashed with dioxane/water (1:1, 20 mL)
5. dry with materialwater (50 mL), and dried in vacuo
6. customThe solid was recrystallized from chloroform
7. customto yield 4.16 g, m.p. 147°-150° C.