反应详情

温度

80 °C

A mixture of K2CO3 (0.238 g, 1.722 mmol), 6-amino-4-methyl-2,10-dihydro-9-oxa-1,2,4a-triaza-phenanthren-3-one (Preparation #2, Step E, 0.20 g, 0.861 mmol), and 1-benzhydryl-3-methylazetidin-3-yl methanesulfonate (Preparation #3, Step B, 0.428 g, 1.292 mmol) in propan-2-ol (10 ml) was stirred at 80° C. overnight. The solution was concentrated in vacuo and the residue was purified by column chromatography on silica gel (eluting with 0 to 50% EtOAc in petroleum ether) to give 6-(1-benzhydryl-3-methyl-azetidin-3-ylamino)-4-methyl-2,10-dihydro-9-oxa-1,2,4a-triaza-phenanthren-3-one (0.234 g, 58%). LC/MS (Table 1, Method 2) Rt=0.948 min; MS m/z: 468 [M+H]+.

1. concentrationThe solution was concentrated in vacuo
2. customthe residue was purified by column chromatography on silica gel (eluting with 0 to 50% EtOAc in petroleum ether)