反应详情

Crude ethyl-[2-amino-3-nitro-6-(trifluoromethyl)-pyridin-4-yl]-benzylcarbamate (65 gm, 170 mmol) was dissolved in ethanol (1000 mL) and 10% Pd—C (6 g m) was added. Hydrogenation at 40° C. and 40 psi for 1 hour gave complete reduction of the nitro group. The catalyst was removed by filtration and the filtrate evaporated to dryness under reduced pressure to give a light brown semi-solid. Trituration with t-butyl methyl ether (150 mL) followed by filtration and washing with the same solvent (30 mL) gave ethyl-[2,3-diamino-6-(trifluoromethyl)-pyridin-4-yl]-benzylcarbamate (36 gm, 60% yield) as a white solid.

1. customHydrogenation at 40° C. and 40 psi for 1 hour gave complete reduction of the nitro group
2. customThe catalyst was removed by filtration
3. customthe filtrate evaporated to dryness under reduced pressure
4. customto give a light brown semi-solid
5. filtrationTrituration with t-butyl methyl ether (150 mL) followed by filtration
6. washwashing with the same solvent (30 mL)