反应详情

温度

2.5 °C

To a suitable reactor was added 4a (2 g, 6.18 mmol), CH2Cl2 (20 mL), DMAP (0.15 g, 1.24 mmol), and Et3N (1.37 g, 13.61 mmol) at 20-30° C. under N2. The mixture was cooled to 0-5° C., and MsCl (1.4 g, 12.36 mmol) in CH2Cl2 (3 mL) solution was added at this temperature. The mixture was warmed to 20-30° C. and stirred for 1 hr. H2O (10 mL) was added at 20-30° C., and the mixture was stirred at this temperature for 30 min. The separated organic portion was washed with 20% NaCl aqueous solution (10 mL). The separated organic portion was concentrated at 40-50° C. under reduced pressure to afford 5 (2.8 g) as a yellow solid in quantitative yield.

1. temperatureThe mixture was warmed to 20-30° C.
2. stirringthe mixture was stirred at this temperature for 30 min
3. washThe separated organic portion was washed with 20% NaCl aqueous solution (10 mL)
4. concentrationThe separated organic portion was concentrated at 40-50° C. under reduced pressure