反应详情

To 3-[4-(3-cyclopentyloxy-4-methoxyphenyl)-piperidin-1-yl]-3-oxo-propionic acid methyl ester (5.3 mmol, 2.0 g) was added a solution of HCl/Et2O (1N, 55 mL) and isoamyl nitrite (6.36 mmol, 0.854 mL) at room temperature. After 10 minutes, the reaction mixture had become homogenous, and a white precipitate formed after and additional 30 minutes. After 3 hours, the reaction mixture was diluted with EtOAc and washed with H2O. The aqueous phase was extracted with EtOAc, the organics dried (Na2SO2) and concentrated in vacuo. The residue was triturated in Et2O/hexane to yield the title compound as a white solid, mp=159°-160° C. (4.7 mmol, 1.89 g, 88%).

1. customa white precipitate formed after and additional 30 minutes
2. waitAfter 3 hours
3. washwashed with H2O
4. extractionThe aqueous phase was extracted with EtOAc
5. dry with materialthe organics dried (Na2SO2)
6. concentrationconcentrated in vacuo
7. customThe residue was triturated in Et2O/hexane