反应详情

0.80 g of 5% platinum carbon (dry) was added to a toluene (80 mL) suspension of 3-benzyloxy-N-methyl-2-nitroaniline (7.19 g, 27.8 mmol), and catalytic hydrogenation reaction was performed under ordinary pressure. The reaction solution was filtered to remove a catalyst, and the catalyst was washed with toluene (10 mL). The washing liquid was added to the precedent filtrate. A 1N hydrochloric acid ethanol solution (28 mL, 28.0 mmol) was added to the mixture under ice cooling, and the mixture was stirred under the same temperature for 30 minutes. The solvent was distilled off under reduced pressure at 20° C. or less. Precipitated crystals were collected by filtration, washed with toluene (15 mL), and dried at 40° C., thereby obtaining 6.30 g of an orange, crystal target compound (yield: 85%).

1. filtrationThe reaction solution was filtered
2. customto remove a catalyst
3. washthe catalyst was washed with toluene (10 mL)
4. additionThe washing liquid was added to the precedent filtrate
5. distillationThe solvent was distilled off under reduced pressure at 20° C. or less
6. customPrecipitated crystals
7. filtrationwere collected by filtration
8. washwashed with toluene (15 mL)
9. customdried at 40° C.