反应详情

温度

70 °C

To a solution of 12-chloro-4-iodo-9-oxa-3,6,13-triazatricyclo[8.4.0.02,6]tetradeca-1(14),2,4,10,12-pentaene (10.0 g, 28.7 mmol) in dry DMF (300 mL) was added Pd(PPh3)2Cl2 (1.00 g, 1.44 mmol) and (Me3Si)2NH (86.1 mmol, 14.0 g). The mixture was stirred at 70° C. for 4 h under carbon monoxide atmosphere. After removal of the solvent, the residue was treated with ice-water. The solid was collected by filtration, dissolved in ethyl acetate (400 ml), dried over anhydrous Na2SO4, and concentrated to give 12-chloro-9-oxa-3,6,13-triazatricyclo[8.4.0.02,6]tetradeca-1(14),2,4,10,12-pentaene-4-carboxamide (7.20 g, 97% yield), which was used in the next step without further purification. LCMS (ESI) m/z: 265.1 [M+H+]

1. customAfter removal of the solvent
2. additionthe residue was treated with ice-water
3. filtrationThe solid was collected by filtration
4. dissolutiondissolved in ethyl acetate (400 ml)
5. dry with materialdried over anhydrous Na2SO4
6. concentrationconcentrated