反应详情

温度

120 °C

A pressure vessel (250 mL flask) containing the compound of Example 1A (10.0 g, 20 mmol) was charged with ethylene glycol (20 mL) and pyridine (4 mL) at ambient temperature, sealed and then heated at 120° C. for 4 hours. The reaction was cooled to ambient temperature, diluted with EtOAc (50 mL), and quenched with 1N HCl (30 mL). The layers were separated and the organic layer was washed with 1N HCl (2×30 mL), dried (Na2SO4), and concentrated. Purification by silica gel chromatography (10%—>40% acetone/hexanes) provided the title compound (3.5 g, 37%). MS (ESI) m/e 484 (M+NH4)+

1. customsealed
2. temperatureThe reaction was cooled to ambient temperature
3. customquenched with 1N HCl (30 mL)
4. customThe layers were separated
5. washthe organic layer was washed with 1N HCl (2×30 mL)
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated
8. customPurification by silica gel chromatography (10%—>40% acetone/hexanes)