反应详情

温度

100 °C

To a suspension of 4-(1-t-butoxycarbonyl-2-methylpiperidin-4-yloxy)-3-chloronitrobenzene (1.15 g) obtained in reference example 85 in 90% formic acid (3.10 g) was added 37% formaldehyde (2.50 g), and the resulting mixture was stirred at 100° C. for 2 hours. After cooling to room temperature, the reaction mixture was neutralized with an aqueous potassium carbonate 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 (9:1) as the eluent to afford the title compound (0.80 g, yield: 90%) 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