反应详情

温度

50 °C

The above ester (0.83 g, 0.002 mol) was dissolved in a mixture of ethanol (8 ml), water (2 ml) and sodium hydroxide (0.58 g, 0.015 mol). The reaction mixture was stirred at room temperature for 50 h and at 50° C. for 5 h. Water. (50 ml) and concentrated hydrochloric acid (3 ml) were added, and the resulting mixture was extracted with dichloromethane (3×10 ml). The combined organic extracts were washed with brine (2×20 ml), dried (MgSO4) and concentrated in vacuo. The residue was re-dissolved in methanol (2 ml) and ethyl acetate (5 ml) and concentrated in vacuo. The solid residue was washed with a small amount of ethyl acetate and dried, affording 0.6 g (73%) of the title compound as a powder.

1. extractionthe resulting mixture was extracted with dichloromethane (3×10 ml)
2. washThe combined organic extracts were washed with brine (2×20 ml)
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. dissolutionThe residue was re-dissolved in methanol (2 ml)
6. concentrationethyl acetate (5 ml) and concentrated in vacuo
7. washThe solid residue was washed with a small amount of ethyl acetate
8. customdried