反应详情

A mixture of the product from part (i) (100 mg) and 5% palladium/carbon (25 mg) in ethanol (25 ml) and acetic acid (25 ml) was hydrogenated at 3.5 bars at room temperature for 3 hours. The catalyst was filtered off, the filtrate was evaporated and the residue was chromatographed on silica gel. Elution with dichloromethane/ethanol (19:1) gave some impurity and further elution with dichloromethane/ethanol/concentrated aqueous ammonia (90:10:1) gave the pure product. The combined product-containing fractions were evaporated to give the title compound as a monohydrate, m.p. 290°-295° (with decomp).

1. filtrationThe catalyst was filtered off
2. customthe filtrate was evaporated
3. customthe residue was chromatographed on silica gel
4. washElution with dichloromethane/ethanol (19:1)
5. customgave
6. washsome impurity and further elution with dichloromethane/ethanol/concentrated aqueous ammonia (90:10:1)
7. customgave the pure product
8. additionThe combined product-containing fractions
9. customwere evaporated