反应详情

A mixture of Example 19B (490 mg, 1.799 mmol), guanidine nitrate (439 mg, 3.60 mmol), and potassium carbonate (497 mg, 3.60 mmol) in DMF (4 mL) was heated overnight at 120° C. After this time, the mixture was cooled to room temperature, then poured into 50 mL of water. The pH was adjusted to about 5 with acetic acid, then the precipitate was collected by filtration, washed with water, and air-dried. The sample was further dried azeotropically with toluene to yield the title compound. 1H NMR (300 MHz, DMSO-d6) δ 10.70 (br, 1H), 7.07-7.20 (m, 4H), 6.14 (br s, 2H), 3.58 (d, J=16.0 Hz, 2H), 2.95 (m, 1H), 2.90 (m, 1H), 2.57-2.66 (m, 2H), 1.59-1.74 (m, 4H), 1.49 (m, 2H). MS (DCI+) m/z 282 (M+H).

1. filtrationthe precipitate was collected by filtration
2. washwashed with water
3. customair-dried
4. dry with materialThe sample was further dried azeotropically with toluene