反应详情

温度

140 °C

A mixture of 5-[3,5-bis(trifluoromethyl)benzyl]-9-chloro-6-oxo-7-phenyl-2,3,4,5-tetrahydro-6H-pyrido[2,3-b][1,5]oxazocine (40.0 mg) and 4-(t-butoxycarbonylamino)piperidine (38.9 mg) was stirred at 140° C. for 5 hours. To the remaining product, water was added and the mixture was extracted with ethyl acetate, followed by drying on anhydrous sodium sulfate. The solvent was then removed to obtain a residue. To this residue, a 3 mol/L ethyl acetate solution of hydrogen chloride (1 mL) was added and the mixture was stirred at room temperature for 1 hour. The solvent was again removed to obtain a residue. To this residue, ethyl acetate was added and the mixture was washed with a saturated aqueous solution of sodium hydrogen carbonate, followed by drying on anhydrous sodium sulfate. The solvent was then removed and the resulting residue was purified on a silica gel column chromatography (ethyl acetate:methanol=3:1) to obtain 9-(4-aminopiperidine-1-yl)-5-[3,5-bis(trifluoromethyl)benzyl]-6-oxo-7-phenyl-2,3,4,5-tetrahydro-6H-pyrido[2,3-b][1,5]oxazocine (35.0 mg, 78%).

1. extractionthe mixture was extracted with ethyl acetate
2. dry with materialby drying on anhydrous sodium sulfate
3. customThe solvent was then removed
4. customto obtain a residue
5. stirringthe mixture was stirred at room temperature for 1 hour
6. customThe solvent was again removed
7. customto obtain a residue
8. washthe mixture was washed with a saturated aqueous solution of sodium hydrogen carbonate
9. dry with materialby drying on anhydrous sodium sulfate
10. customThe solvent was then removed
11. customthe resulting residue was purified on a silica gel column chromatography (ethyl acetate:methanol=3:1)