反应详情

The above ester (6.7 g, 15.9 mmol) was dissolved in ethanol (30 ml) and 20% sodium hydroxide (10 ml) was added. After stirring for 3 days, ethanol was evaporated in vacuo, water (50 ml) and diethyl ether (50 ml) were added and the phases were separated. The water phase was treated with acetic acid and extracted with dichloromethane. The organic phase was dried (MgSO4) and the solvent was evaporated in vacuo. The residue (7.0 g) was dissolved in acetone (30 ml) and treated with a solution of oxalic acid dihydrate (2.0 g) in acetone (10 ml). The precipitate was filtered off and dried, affording 6.1 g (77%) of the title compound.

1. customethanol was evaporated in vacuo, water (50 ml) and diethyl ether (50 ml)
2. additionwere added
3. customthe phases were separated
4. additionThe water phase was treated with acetic acid
5. extractionextracted with dichloromethane
6. dry with materialThe organic phase was dried (MgSO4)
7. customthe solvent was evaporated in vacuo
8. dissolutionThe residue (7.0 g) was dissolved in acetone (30 ml)
9. additiontreated with a solution of oxalic acid dihydrate (2.0 g) in acetone (10 ml)
10. filtrationThe precipitate was filtered off
11. customdried