反应详情

温度

10 °C

A mixture of wet crystals of 4-(acetylamino)-3-nitrobenzoate (45.3 g, purity: 66.2%), ethanol (191.6 g), water (31.9 g), and palladium-on-carbon (palladium content: 5%, water content: 50%, 3.0 g) was stirred at 40° C. for 19 hours at a hydrogen atmosphere. The catalyst was collected by filtration and washed with a mixed solvent of water and ethanol (1/9, 30.0 g). The filtrate was concentrated, and t-butyl methyl ether (33.0 g) was added dropwise thereto at 50° C., and the mixture was cooled to 10° C. to effect crystallization. Crystals were collected and washed with t-butyl methyl ether (30.0 g), and dried at 60° C. under reduced pressure. Thus, ethyl 4-(acetylamino)-3-aminobenzoate (18.2 g) was obtained.

1. filtrationThe catalyst was collected by filtration
2. washwashed with a mixed solvent of water and ethanol (1/9, 30.0 g)
3. concentrationThe filtrate was concentrated
4. additiont-butyl methyl ether (33.0 g) was added dropwise
5. customcrystallization
6. customCrystals were collected
7. washwashed with t-butyl methyl ether (30.0 g)
8. customdried at 60° C. under reduced pressure