反应详情

In DMF (800 ml), 39.23 g (85.75 mmol) of the compound from Example 10A were introduced and then 4 g of palladium (10% on carbon) were added. The mixture was hydrogenated with stirring overnight under standard hydrogen pressure. The batch was filtered over kieselguhr and the filter product was washed with a little DMF and then with a little methanol, and concentrated to dryness. The residue was admixed with ethyl acetate and stirred vigorously, and the precipitate was filtered off with suction, washed with ethyl acetate and diisopropyl ether and dried under a high vacuum over Sicapent.

1. filtrationThe batch was filtered over kieselguhr
2. washthe filter product was washed with a little DMF
3. concentrationwith a little methanol, and concentrated to dryness
4. stirringstirred vigorously
5. filtrationthe precipitate was filtered off with suction
6. washwashed with ethyl acetate and diisopropyl ether
7. customdried under a high vacuum over Sicapent