反应详情

A solution of codeine or codeine phosphate was dissolved in the appropriate solvent system and a specified volume of hydrochloric acid of varying concentration was added. Manganese dioxide (either freshly prepared γ-manganese dioxide or activated manganese dioxide from Aldrich) was added and the reaction mixture was stirred at ambient temperature for 1.5 to 4 hours. The progress of the reaction was monitored by HPLC. The reaction mixture was filtered through a celite pad, washed with additional solvent or water, and neutralised with ammonium hydroxide. The product was extracted with methylene chloride (3×150 ml) and the combined extracts washed with water and dried over anhydrous sodium sulphate. The organic layer was then evaporated to yield codeinone.

1. concentrationconcentration
2. additionwas added
3. additionManganese dioxide (either freshly prepared γ-manganese dioxide or activated manganese dioxide from Aldrich) was added
4. filtrationThe reaction mixture was filtered through a celite pad
5. washwashed with additional solvent or water
6. extractionThe product was extracted with methylene chloride (3×150 ml)
7. washthe combined extracts washed with water
8. dry with materialdried over anhydrous sodium sulphate
9. customThe organic layer was then evaporated