反应详情

(±)-Phenylmethyl-[1-(acetyloxymethyl)-2-oxo-2-(1H-pyrrol-1-ylamino)ethyl]carbamate (4.18 g) was dissolved in 100 ml of methanol and 5% Pd/C (450 mg) was added. The solution was hydrogenated at atmospheric pressure and room temperature until absorption of 90% of the theoretical amount of hydrogen. The catalyst was removed by filtration and the filtrate was evaporated to dryness. The residue was purified by flash column chromatography (silica gel, ethyl acetate/methanol, 19:1) and the desired fractions combined and evaporated. Recrystallization of the residue from ethyl acetate/methanol/hexane afforded the product obtained as a powder (1.24 g), m.p. 147°-148° C.

1. customThe solution was hydrogenated at atmospheric pressure and room temperature until absorption of 90% of the theoretical amount of hydrogen
2. customThe catalyst was removed by filtration
3. customthe filtrate was evaporated to dryness
4. customThe residue was purified by flash column chromatography (silica gel, ethyl acetate/methanol, 19:1)
5. customevaporated
6. customRecrystallization of the residue from ethyl acetate/methanol/hexane
7. customafforded the product