反应详情

8.56 g (36.7 mmol) of 2-(3-cyano-phenoxy)-2-methyl-propionic acid ethyl ester was dissolved in 65 ml ethanol; then, 6.5 ml acetic acid was added, followed by 0.9 g Pd—C (10%) and the reaction mixture was hydrogenated under 1 atm of H2-pressure during 5 hours. Then, it was filtered (Celite), the filter cake was washed twice with ethanol and the solvents were evaporated. The residue was partitioned between crashed ice/1N NaOH/EtOAc and extracted twice with EtOAc; the organic phases were washed with water, dried (MgSO4) and evaporated. The crude product was purified by flash chromatography (SiO2, MeCl2/MeOH) to give 7.71 g of the title compound as colorless oil.

1. filtrationThen, it was filtered (Celite)
2. washthe filter cake was washed twice with ethanol
3. customthe solvents were evaporated
4. customThe residue was partitioned
5. extractionextracted twice with EtOAc
6. washthe organic phases were washed with water
7. dry with materialdried (MgSO4)
8. customevaporated
9. customThe crude product was purified by flash chromatography (SiO2, MeCl2/MeOH)