反应详情

A mixture of 5.0 gm (16.3 mMol) 3-(naphth-2-yl)-8-ethoxycarbonyl-8-azabicyclo[3.2.1]oct-2-ene, 4.07 gm (81.3 mMol) hydrazine hydrate, and 5.49 gm (97.8 mMol) potassium hydroxide in 120 mL ethylene glycol was heated at reflux for 2 hours. The reaction mixture was allowed to cool gradually to room temperature. After 16 hours the reaction mixture was poured into water and extracted well with diethyl ether. The organic phase was dried over sodium sulfate and concentrated under reduced pressure. The residue was dissolved in 1N hydrochloric acid and the solution washed with diethyl ether. The aqueous phase was basified and the mixture extracted well with ethyl acetate. The organic phase was dried over sodium sulfate and concentrated under reduced pressure to provide the title compound as a yellow oil.

1. temperaturewas heated
2. temperatureat reflux for 2 hours
3. extractionextracted well with diethyl ether
4. dry with materialThe organic phase was dried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. dissolutionThe residue was dissolved in 1N hydrochloric acid
7. washthe solution washed with diethyl ether
8. extractionthe mixture extracted well with ethyl acetate
9. dry with materialThe organic phase was dried over sodium sulfate
10. concentrationconcentrated under reduced pressure