反应详情

温度

100 °C

To a solution of tert-butyl 3-((8-bromo-1-methyl-2-oxo-1,2,3,5-tetrahydrobenzo[5,6][1,4]oxazino[3,4-c][1,2,4]triazin-9-yl)amino)azetidine-1-carboxylate (Example 1, Step B, 0.20 g, 0.43 mmol), (E)-2-(2-ethoxyvinyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (0.1 g, 0.5 mmol) in dioxane (6 mL) and water (1 mL) was added PdCl2(dppf)-CH2Cl2 adduct (0.035 g, 0.043 mmol) and K2CO3 (0.118 g, 0.85 mmol). The reaction mixture was stirred at 100° C. overnight. The reaction mixture was cooled to ambient temperature, the solvent was removed in vacuo and the residue was purified by chromatography on silica gel (eluting with 2% MeOH in DCM) to give (E)-tert-butyl 3-((8-(2-ethoxyvinyl)-1-methyl-2-oxo-1,2,3,5-tetrahydrobenzo[5,6][1,4]oxazino[3,4-c][1,2,4]triazin-9-yl)amino)azetidine-1-carboxylate (0.10 g, 51%) as a yellow solid. LC/MS (Table 1, Method 2) Rt=1.352 min.; MS m/z: 458 [M+H]+.

1. temperatureThe reaction mixture was cooled to ambient temperature
2. customthe solvent was removed in vacuo
3. customthe residue was purified by chromatography on silica gel (eluting with 2% MeOH in DCM)