反应详情

温度

2.5 °C

To the solution of 14-hydroxycodeinone produced in Example 5 is added 0.5 g of 5% palladium on carbon, 50% wet. The mixture is hydrogenated at 30 to 40 psi for a period of 18 to 25 hours at ambient temperature. The catalyst is filtered off and is washed with 5 ml of water. The filtrate is cooled to 0-5° C. and with stirring, sufficient concentrated (28-30%) ammonium hydroxide is added to raise the pH to 10-12. The resulting suspension is stirred at 0-5° C. for 1-2 hours. The solid is filtered off and is washed with two 5 ml portions of water. The product is dried in vacuo (e.g., 50 mm Hg) at 30-40° C. to yield 8.1 g of oxodone (85% yield based on thebaine bitartrate). The product purity is better than 98%.

1. filtrationThe catalyst is filtered off
2. washis washed with 5 ml of water
3. concentrationsufficient concentrated (28-30%) ammonium hydroxide
4. additionis added
5. temperatureto raise the pH to 10-12
6. stirringThe resulting suspension is stirred at 0-5° C. for 1-2 hours
7. filtrationThe solid is filtered off
8. washis washed with two 5 ml portions of water
9. customThe product is dried in vacuo (e.g., 50 mm Hg) at 30-40° C.
10. customto yield 8.1 g of oxodone (85% yield based on thebaine bitartrate)