反应详情

A solution of Example 10B (4.5 g, 21.4 mmol), guanidine hydrochloride (6.13 g, 64.2 mmol), and potassium carbonate (9.46 g, 68.5 mmol) in N,N-dimethylformamide (30 mL) was heated at 105-110° C. for 3 hours. The mixture was then filtered through a layer of diatomaceous earth, and the filter pad was washed with a small amount of N,N-dimethylformamide. Approximately two volumes of water were then added, and the pH of the resulting mixture was adjusted to pH 6-7 with acetic acid. The precipitate was collected, washed with water, and dried under vacuum to provide the title product. 1H NMR (300 MHz, DMSO-d6) δ 10.50-10.61 (m, 1H), 5.98-6.08 (m, 2H), 2.20 (t, 2H), 1.95-2.04 (m, 2H), 1.68-1.76 (m, 2H), 1.61-1.68 (m, 2H), 1.48-1.58 (m, 4H), 1.34-1.45 (m, 2H); MS (DCI+) m/z 220 (M+H)+.

1. filtrationThe mixture was then filtered through a layer of diatomaceous earth
2. washthe filter pad was washed with a small amount of N,N-dimethylformamide
3. additionApproximately two volumes of water were then added
4. customThe precipitate was collected
5. washwashed with water
6. customdried under vacuum