反应详情

1.22 g (approx. 3.34 mmol, purity approx. 60%) of the compound from example 42A were initially charged in pyridine (149 ml) and then 505 mg (0.47 mmol) of palladium (10% on charcoal) were added. The mixture was hydrogenated under standard hydrogen pressure at RT overnight. The reaction mixture was then filtered through kieselguhr and the filtercake was washed with methanol. The filtrate was concentrated, methanol was added and the solids were filtered off. The filtrate was concentrated by rotary evaporation, the residue was chromatographed on silica gel (eluent: 5:1, 3:1 cyclohexane/ethyl acetate) and the product fractions were concentrated. This gave 491 mg (44% of theory) of the title compound.

1. customat RT
2. customovernight
3. filtrationThe reaction mixture was then filtered through kieselguhr
4. washthe filtercake was washed with methanol
5. concentrationThe filtrate was concentrated
6. additionmethanol was added
7. filtrationthe solids were filtered off
8. concentrationThe filtrate was concentrated by rotary evaporation
9. customthe residue was chromatographed on silica gel (eluent: 5:1, 3:1 cyclohexane/ethyl acetate)
10. concentrationthe product fractions were concentrated