反应详情

A mixture of 3-(7-bromo-4-methyl-3-oxo-2,3,4,10-tetrahydro-9-oxa-1,2,4a-triaza-phenanthren-6-yloxy)-azetidine-1-carboxylic acid tert-butyl ester (Example #65, Step G, 0.030 g, 0.064 mmol), isopropenyl boronic acid (0.032 g, 0.193 mmol), K2CO3 (0.018 g, 0.13 mmol) and Pd(dppf)Cl2.CH2Cl2 (0.011 g, 0.013 mmol) in dioxane (3 mL) and H2O (0.5 mL) was stirred at 80° C. for 15 h. The mixture was cooled to ambient temperature and the solvent was removed in vacuo. The residue was purified by preparative TLC (eluting with 20% EtOAc in petroleum ether) to give 3-(7-isopropenyl-4-methyl-3-oxo-2,3,4,10-tetrahydro-9-oxa-1,2,4a-triaza-phenanthren-6-yloxy)-azetidine-1-carboxylic acid tert-butyl ester as a white solid (0.09 g, 33%). LC/MS (Table 1, Method 2) Rt=1.241 min.; MS m/z: 429 [M+H]+.

1. customthe solvent was removed in vacuo
2. customThe residue was purified by preparative TLC (eluting with 20% EtOAc in petroleum ether)