反应详情

温度

115 °C

In a 25-ml flask, 2′-bromo-7′-hydroxyspiro[morpholine-3,9′-xanthen]-5-one (0.020 g, 0.055 mmol) was dissolved in DMF (1 mL). Cesium carbonate (0.043 g, 0.133 mmol) was added, followed by 1-iodo-2,2-dimethylpropane (0.022 g, 0.110 mmol). The reaction was heated in a 115° C. oil bath for 10 h. The reaction was cooled to ambient temperature and concentrated. The residue was taken up in 0.3 M aqueous HCl (15 mL) and the aqueous layer was extracted with EtOAc (3×20 mL). The organic layers were combined, washed with saturated brine (5 mL), dried over sodium sulfate, and concentrated. The residue was purified by chromatography (25% EtOAc/hexane) to afford (R)-2′-bromo-7′-(neopentyloxy)spiro[morpholine-3,9′-xanthen]-5-one.

1. temperatureThe reaction was cooled to ambient temperature
2. concentrationconcentrated
3. extractionthe aqueous layer was extracted with EtOAc (3×20 mL)
4. washwashed with saturated brine (5 mL)
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customThe residue was purified by chromatography (25% EtOAc/hexane)