反应详情

温度

50 °C

To a solution of the compound of Example 1-3 (1.76 g, 3.34 mmol) in tert-butyl alcohol (34 mL) was added potassium hydroxide (1.76 g, 31.4 mmol), and the mixture was stirred at 50° C. for 1.5 hours. To the reaction solution were added ethyl acetate (100 mL) and water (2 mL), and then the mixture was dried over magnesium sulfate and filtered. The mixture was evaporated, and then dissolved in ethyl acetate again and filtered. The filtrate was evaporated, and then thereto were added tetrahydrofuran (100 mL) and 1M hydrochloric acid (5 mL), and the mixture was evaporated, and then the residual water was removed by azeotropic distillation with toluene. The resulting solid was washed with diethyl ether, and then dried to give the titled compound (1.89 g, 97%).

1. dry with materialthe mixture was dried over magnesium sulfate
2. filtrationfiltered
3. customThe mixture was evaporated
4. dissolutiondissolved in ethyl acetate again
5. filtrationfiltered
6. customThe filtrate was evaporated
7. additionwere added tetrahydrofuran (100 mL) and 1M hydrochloric acid (5 mL)
8. customthe mixture was evaporated
9. customthe residual water was removed by azeotropic distillation with toluene
10. washThe resulting solid was washed with diethyl ether
11. customdried