反应详情

To a solution of (S)-5-tert-butyl 6-methyl 5-azaspiro[2.4]heptane-5,6-dicarboxylate (0.436 g, 1.708 mmol) in ethanol (4 mL) was added a solution of LiOH.H2O (86.0 mg, 2.049 mmol, 1.2 eq) in H2O (2 mL) at room temperature. The mixture was stirred at room temperature for 20 hours. EtOH was removed by rotavapor. The aqueous residue was diluted with H2O and extracted with Et2O. The aqueous layer was cooled with an ice bath and acidified to pH ˜2 with 1 N HCl. The resulting milky solution was extracted with a mixed solvent of EtOAc and CH2Cl2. The organic layer was dried (Na2SO4), filtered and evaporated. The residue was dried under vacuum to afford the desired product as an off-white solid (0.422 g, 100%).

1. customEtOH was removed by rotavapor
2. additionThe aqueous residue was diluted with H2O
3. extractionextracted with Et2O
4. temperatureThe aqueous layer was cooled with an ice bath
5. extractionThe resulting milky solution was extracted with a mixed solvent of EtOAc and CH2Cl2
6. dry with materialThe organic layer was dried (Na2SO4)
7. filtrationfiltered
8. customevaporated
9. customThe residue was dried under vacuum