反应详情

A suspension of N-(4-methyl-3-nitro-phenyl)-3-trifluoromethyl-benzamide (9.91 g, 30.6 mmol) and 10% palladium on charcoal (990 mg) in ethanol (180 ml) is hydrogenated at atmospheric pressure and room temperature. After 2 h the reaction is complete, the catalyst is removed by filtration through Celite, and the filtrate is evaporated to dryness. Recrystallization of the crude product from ethyl acetate/hexanes followed by vacuum drying at 45° C. overnight affords the title compound as fluffy light grey needles: HPLC: tR=5.38 min (purity: >99%, gradient A), ESI-MS: 295.3 [MH]+

1. customis hydrogenated at atmospheric pressure and room temperature
2. customthe catalyst is removed by filtration through Celite
3. customthe filtrate is evaporated to dryness
4. customRecrystallization of the crude product from ethyl acetate/hexanes
5. customdrying at 45° C. overnight