反应详情

温度

150 °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-(pyrrolidine-1-yl)piperidine (30.0 mg) was stirred at 150° C. for 3 hours. To the remaining product, water was added and the mixture was extracted with ethyl acetate. The extract was then washed with a saturated aqueous solution of sodium hydrogen carbonate and was dried on anhydrous sodium sulfate. The solvent was removed and the resulting residue was purified on a silica gel column chromatography (ethyl acetate:methanol=3:1) to obtain 5-[3,5-bis(trifluoromethyl)benzyl]-6-oxo-7-phenyl-9-[4-(pyrrolidine-1-yl)piperidine-1-yl]-2,3,4,5-tetrahydro-6H-pyrido[2,3-b][1,5]oxazocine (25.0 mg, 51%).

1. extractionthe mixture was extracted with ethyl acetate
2. washThe extract was then washed with a saturated aqueous solution of sodium hydrogen carbonate
3. dry with materialwas dried on anhydrous sodium sulfate
4. customThe solvent was removed
5. customthe resulting residue was purified on a silica gel column chromatography (ethyl acetate:methanol=3:1)