反应详情

To a solution of diethyl 4-(5-(2-(4-hydroxy-2-(pyridazin-3-yl)pyrimidine-5-carboxamido) propan-2-yl)pyridin-2-yl)phenylphosphonate (180 mg, 0.33 mmol) in DCM (5 ml) was added dropwise TMSBr (1.50 g, 9.85 mmol) at 0° C., the reaction mixture was stirred at room temperature for overnight. Then evaporated the solution and diluted with 20 ml MeOH, and stirred at room temperature for 30 mins, concentrated under vacuo, purified by Pre-HPLC to give product 33-1. 1H NMR (CDCl3-d6, 300 MHz,): δ 9.50 (s, 1H), 8.71 (s, 1H), 8.50 (d, 1H), 8.11 (m, 2H), 7.72-8.02 (m, 5H), 3.15 (s, 1H), 1.76 (s, 6H). (M+H)+=493.1.

1. customThen evaporated the solution
2. additiondiluted with 20 ml MeOH
3. stirringstirred at room temperature for 30 mins
4. concentrationconcentrated under vacuo
5. custompurified by Pre-HPLC