反应详情

温度

60 °C

The compound (6.2 g) obtained in Example 310 is dissolved in methylene chloride (120 ml), a 1 mol/L ethanol solution (11.28 ml) of p-toluenesulfonic acid was added to the solution, and the solvent was distilled off. Ethanol (95 ml) containing 15% water was added to the residue, and the mixture was stirred at 60° C. to dissolve it. The solution was then cooled to room temperature and stirred for a day. Crystals deposited were collected by filtration, washed with ethanol and dried at room temperature for 2 hours under reduced pressure to obtain the title compound (7.4 g).

1. distillationthe solvent was distilled off
2. additionEthanol (95 ml) containing 15% water
3. additionwas added to the residue
4. dissolutionto dissolve it
5. temperatureThe solution was then cooled to room temperature
6. stirringstirred for a day
7. filtrationCrystals deposited were collected by filtration
8. washwashed with ethanol
9. customdried at room temperature for 2 hours under reduced pressure