反应详情

温度

10 °C

Additional trials were conducted in which the wt % of the catalyst was varied, the wt % of H2SO4 was varied, the presence of various co-catalysts were tested, and reaction times were varied. Table 1 lists the various reaction parameters. For each trial, a reaction flask was charged with morphine, EtOH, and water (the ratio of morphine to EtOH to water was 1 g:1.6-2 mL:0.8-1 mL). The reaction mixture was stirred and the flask was charge with catalyst (RuCl3.xH2O), acid (if applicable), and co-catalyst (if applicable). The reaction mixture was heated to reflux under nitrogen for the indicated period of time. The reaction was monitored by UHPLC. Upon completion of the reaction, the reaction flask was charged with anti-solvent, the pH of the mixture was adjusted, and the mixture was cooled to room temperature or 10° C. to precipitate the product. The mixture was filtered to give hydromorphone sulfate or hydromorphone base. The purity of the product was checked using orthogonal HPLC methods.

1. customreaction times
2. customthe various reaction parameters
3. temperatureThe reaction mixture was heated
4. temperatureto reflux under nitrogen for the indicated period of time
5. customUpon completion of the reaction
6. additionthe reaction flask was charged with anti-solvent, the pH of the mixture
7. customto precipitate the product
8. filtrationThe mixture was filtered