反应详情

A mixture of 2.6 g of the diester (4), of 10% Pd on charcoal and 75 mL of dioxane were shaken under 50 psi of hydrogen for 17 hours at 50° C. The catalyst was removed by filtering through Celite and the solvent was removed. The residue was chromatographed on 200 g of silica gel eluting with 3:17 (v/v) acetone: CH2Cl2. Fractions 75-120 (17 mL/fraction) were combined and concentrated to yield 0.5 g of a white powder. Recrystallization from MeOH-H2O produced an analytical sample, m.p. 171°-172° C.

1. customThe catalyst was removed
2. filtrationby filtering through Celite
3. customthe solvent was removed
4. customThe residue was chromatographed on 200 g of silica gel eluting with 3:17 (v/v) acetone
5. concentrationconcentrated