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)-3-methyl-azetidine-1-carboxylic acid tert-butyl ester (Example #82, Step A, 0.032 g, 0.066 mmol), 2,4,6-trimethyl-cyclotriboroxane (0.025 g, 0.199 mmol), K2CO3 (0.018 g, 0.133 mmol) and Pd(dppf)Cl2.CH2Cl2 (0.006 g, 0.007 mmol) in dioxane (3 mL) and water (0.5 mL) was stirred at 110° C. for 4 h. The solvent was removed in vacuo and the residue was purified by preparative TLC (eluting with 30% EtOAc in petroleum ether) to give 3-(4,7-dimethyl-3-oxo-2,3,4,10-tetrahydro-9-oxa-1,2,4a-triaza-phenanthren-6-yloxy)-3-methyl-azetidine-1-carboxylic acid tert-butyl ester as a white solid (0.024 g, 87%). LC/MS (Table 1, Method 2) Rt=1.160 min.; MS m/z: 417 [M+H]+.

1. customThe solvent was removed in vacuo
2. customthe residue was purified by preparative TLC (eluting with 30% EtOAc in petroleum ether)