反应详情

4-Morpholin-4-yl-butyric acid ethyl ester (about 25 mmol) was suspended in 100 mL of NaOH 10%, and the mixture was heated at reflux for 10 hours. The reaction mixture was then allowed to cool down to room temperature and washed with AcOEt. The aqueous layer was recovered by extraction and acidified at 0° C. with HCl 37% to pH 4 and concentrated under reduced pressure. The residue was treated with EtOH and the sodium chloride which precipitated was filtered off. The crude was treated with acetone and filtered; evaporation of the solvent under reduced pressure afforded 3.2 g of the title compound as a white solid in 72% overall yield of steps a) and b).

1. temperaturethe mixture was heated
2. temperatureat reflux for 10 hours
3. washwashed with AcOEt
4. customThe aqueous layer was recovered by extraction
5. customacidified at 0° C. with HCl 37% to pH 4
6. concentrationconcentrated under reduced pressure
7. additionThe residue was treated with EtOH
8. customthe sodium chloride which precipitated
9. filtrationwas filtered off
10. additionThe crude was treated with acetone
11. filtrationfiltered
12. customevaporation of the solvent under reduced pressure