反应详情

A solution of 9.20 g (23.4 mmol, purity 75%) of the compound from Example 52A in concentrated acetic acid (192 ml) was admixed with 1.94 g of palladium/carbon (10% palladium) and 2.23 g of platinum (IV) oxide. This was followed by hydrogenation under a hydrogen atmosphere at standard pressure for 6 h, then addition of another 1.00 g of palladium/carbon (10% palladium) and 2.00 g of platinum(IV) oxide, and hydrogenation under a hydrogen atmosphere at standard pressure overnight. Subsequently, a further 1.00 g of palladium/carbon (10% palladium) and 3.00 g of platinum(IV) oxide were added, and hydrogenation was effected under a hydrogen atmosphere at standard pressure for a further 24 h. The reaction solution was filtered through Celite, the filter residue was washed with methanol/water and the combined filtrates were concentrated under reduced pressure. The residue was taken up in dichloromethane and then washed with a 1 N aqueous sodium carbonate solution. The organic phase was dried over sodium sulphate, filtered and concentrated under reduced pressure. Yield: 6.64 g (85% of theory, purity 90%)

1. waithydrogenation was effected under a hydrogen atmosphere at standard pressure for a further 24 h
2. filtrationThe reaction solution was filtered through Celite
3. washthe filter residue was washed with methanol/water
4. concentrationthe combined filtrates were concentrated under reduced pressure
5. washwashed with a 1 N aqueous sodium carbonate solution
6. dry with materialThe organic phase was dried over sodium sulphate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure