反应详情

温度

87.5 °C

To a mixture of 5-methyl-4-oxo-3,4-dihydropyrrolo[2,1-f][1,2,4]triazin-6-yl pivalate (300 mg, 1.20 mmol), phosphorus oxychloride (368 mg mL, 2.4 mmol) and DIEA (0.5 mL, 2.80 mmol) was added acetonitrile (10 mL). The reaction was heated at 85-90° C. for 4 hours and then cooled to room temperature. The mixture was diluted with ethyl acetate (10 mL) and water (5 mL). The organic layer was separated and dried with sodium sulfate, concentrated in vacuo and purified by silica gel flash chromatography (eluted with 1-25% EtOAc/CH2Cl2) to give the title compound (250 mg, 78%) as a white solid.

1. temperaturecooled to room temperature
2. customThe organic layer was separated
3. dry with materialdried with sodium sulfate
4. concentrationconcentrated in vacuo
5. custompurified by silica gel flash chromatography (eluted with 1-25% EtOAc/CH2Cl2)