反应详情

A solution of 1-(1,4-dioxaspiro[4.5]dec-7ylmethyl)-1,2,3,6-tetrahydro-4-phenylpyridine (Step C) (90.4 g) in 500 mL of acetone and 500 mL of 10% aqueous hydrochloric acid solution is refluxed, under nitrogen, for 3 hours. The solvent is evaporated in vacuo and partitioned into ethyl acetate/dilute ammonium hydroxide solution. The organic extract is dried over magnesium sulfate and concentrated, leaving the title compound (68.9 g) as a light pink solid; mp 56°-59° C. Mass spectrum (MS) electron ionization (EI) 269 (m, 41%), 172 (100%).

1. customThe solvent is evaporated in vacuo
2. custompartitioned into ethyl acetate/dilute ammonium hydroxide solution
3. extractionThe organic extract
4. dry with materialis dried over magnesium sulfate
5. concentrationconcentrated