反应详情

Compound (1C) (4.2 g, 15.0 mmol) and urea (9.0 g, 10 eq) were heated to a melt at 160° C. with stirring. After 2 hours, the melt solidified and by TLC the reaction was complete. The reaction mixture was cooled to room temperature, water (250 mL) was added, and the resulting mixture was left to stand for 1 hour. Then the solids were broken up with a spatula and the mixture was stirred vigorously for 1 hour. After suction filtration, a tan powder was collected which was air-dried in the frit for two days. Drying under high vacuum at 56° C. gave the title compound (1D) as a tan powder (4.307 g, (M−H)−=290, M.P.>300° C.).

1. waitthe resulting mixture was left
2. waitto stand for 1 hour
3. stirringthe mixture was stirred vigorously for 1 hour
4. filtrationAfter suction filtration
5. customa tan powder was collected which
6. customwas air-dried in the frit for two days
7. customDrying under high vacuum at 56° C.