反应详情

To a stirred solution of methyl 3,4-dihydroxy-5-nitrobenzoate (11.9 g, 55.8 mmol) in EtOH (200 mL), 4M HCl in dioxane (13.96 mL, 55.8 mmol) and 10% palladium on carbon (4.0 g, 3.76 mmol) were added. The reaction mixture was hydrogenated at atmospheric pressure of H2 for 3 hours (TLC-monitoring). The resulting mixture was filtered and concentrated with the use of a rotary evaporator. The residue was triturated with ether (100 mL). The precipitate was filtered off and vacuum-dried to afford methyl 3-amino-4,5-dihydroxybenzoate hydrochloride (12.0 g, 54.6 mmol, 98% yield).

1. filtrationThe resulting mixture was filtered
2. concentrationconcentrated with the use of a rotary evaporator
3. customThe residue was triturated with ether (100 mL)
4. filtrationThe precipitate was filtered off
5. customvacuum-dried