反应详情

温度

100 °C

To a solution of 12-chloro-9-oxa-3,6,13-triazatricyclo[8.4.0.02,6]tetradeca-1(14),2,4,10,12-pentaene-4-carboxamide (0.380 mmol, 100 mg) in 1,4-dioxane (3 mL) was added DMF-DMA (1.14 mmol, 147 mg). The mixture was stirred at 100° C. for 1 hour under nitrogen atmosphere. Then solvent was evaporated under reduced pressure, the residue was washed by ether to give 12-chloro-N-[(1E)-(dimethylamino)methylidene]-9-oxa-3,6,13-triazatricyclo[8.4.0.02,6]tetradeca-1(14),2,4,10,12-pentaene-4-carboxamide (80 mg, 68% yield), which was used in the next step without further purification. LCMS (ESI) m/z: 320.1 [M+H+]

1. customThen solvent was evaporated under reduced pressure
2. washthe residue was washed by ether