反应详情

A mixture of 18.0 g (50.0 mmol) of 19, 1.8 g of 10% Pd on charcoal, and 180 mL of anhydrous ethanol was hydrogenated in a stainless steel autoclave at 20 atm constant pressure of hydrogen and 80° C. The reaction was carried out for ca. 4 hr, i.e. until hydrogen consumption was finished. The resulting mixture was filtered through glass frit, and the filtrate was evaporated to dryness. The product was isolated from the residue using flash-chromatography on silica gel 60 (40-63 um, eluent: hexanes-ethyl acetate from 50:1 to 2:1, vol.) to yield 13.1 g (73%) of the title product.

1. customi.e. until hydrogen consumption
2. filtrationThe resulting mixture was filtered through glass frit
3. customthe filtrate was evaporated to dryness
4. customThe product was isolated from the residue