反应详情

温度

50 °C

The compound of Example 56 (0.69 g, 1.5 mmol) was put in 10 mL of a MeOH solution to which SnCl2.2H2O (1.37 g, 6.4 mmol) was added, and stirred for 1.5 hours while maintaining the temperature at 50° C. A saturated NaHCO3 aqueous solution was introduced and stirred for 2 hours, and then it was extracted with ethyl acetate. After distillation under reduced pressure, 2,5-dimethoxytetrahydrofuran (0.20 mLo, 1.5 mmol) and 1 mL of acetic acid were introduced and refluxed for 2 hours. 50 mL of ethyl acetate was introduced and the reactant was washed with 50 mL of a saturated NaHCO3 aqueous solution and 50 mL of a 1 N HCl aqueous solution, and dried and then concentrated under reduced pressure. The mixture was separated with hexane and ethyl acetate (3:1) in a silica gel column to obtain a yellow oily title compound (0.19 g, 26%).

1. additionwas added
2. stirringstirred for 2 hours
3. extractionit was extracted with ethyl acetate
4. additionwere introduced
5. temperaturerefluxed for 2 hours
6. washthe reactant was washed with 50 mL of a saturated NaHCO3 aqueous solution and 50 mL of a 1 N HCl aqueous solution
7. customdried
8. concentrationconcentrated under reduced pressure
9. customThe mixture was separated with hexane and ethyl acetate (3:1) in a silica gel column