反应详情

温度

70 °C

To a solution of 4-hydroxy-2-(pyridin-2-yl)pyrimidine-5-carboxylic acid (1-1-h, 1.1 g, 5.1 mmol) in acetonitrile (20 ml) was added Et3N (1.02 g, 10.2 mmol). The mixture was aged for 15 min at room temperature. To the mixture was added CDI (800 mg, 5.1 mmol) and the resulting mixture was heated to 70° C. for 3 h. To the hot homogeneous solution was then added in one portion 4-(amino(4-methoxyphenyl)methyl)phenylphosphinic acid hydrochloride (1-1-e, 1.4 g, 5.1 mmol). Heating was continued for 2 h at 70° C. Then it was concentrated under vacuum and the residue was purified on prep-HPLC to provide the 1-1-6 (160 mg, 6%). 1H NMR (CD3OD, 300 MHz,): δ 13.35 (br, 1H), 8.80 (m, 1H), 8.62 (m, 2H), 8.45 (m, 1H), 7.23 (m, 7H), 7.79 (m, 2H), 6.52 (s, 1H), 6.25 (m, 1H), 3.70 (m, 3H).

1. temperatureHeating
2. waitwas continued for 2 h at 70° C
3. concentrationThen it was concentrated under vacuum
4. customthe residue was purified on prep-HPLC