反应详情

温度

100 °C

To a suspension of 4-(1-t-butoxycarbonylpiperidin-4-yloxy)-3-trifluoromethylnitrobenzene (2.45 g) obtained in reference example 100 in 90% formic acid (8.80 g) was added 37% formaldehyde (5.50 g), and the resulting mixture was stirred at 100° C. for 6 hours. After cooling to room temperature, the reaction mixture was neutralized with an aqueous sodium hydrogencarbonate solution and extracted with ethyl acetate. The extract was washed with a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate and evaporated in vacuo. The residue obtained was purified by chromatography on a silica gel column using a mixed solvent of dichloromethane and methanol (10:1) as the eluent to afford the title compound (1.82 g, yield: 95%) as a yellow oil.

1. temperatureAfter cooling to room temperature
2. extractionextracted with ethyl acetate
3. washThe extract was washed with a saturated aqueous sodium chloride solution
4. dry with materialdried over anhydrous magnesium sulfate
5. customevaporated in vacuo
6. customThe residue obtained
7. customwas purified by chromatography on a silica gel column