反应详情

trans-5-[4-[(t-Butoxycabonyl)methyloxy]cyclohexyl]-1,3-dimethylhexahydro-2-oxo-1,3,5-triazine (300mg, 0.879 mmol) was dissolved in t-butanol (5 ml) and a saturated aqueous ammonium chloride solution (5 ml) was added, which was followed by refluxing under heating for 2 hours. The reaction mixture was adjusted to pH 10 with a 1N aqueous sodium hydroxide solution and extracted with benzene. The extract was washed with water and saturated brine, and dried over anhydrous sodium sulfate. After filtration, low boiling matters were distilled away from the filtrate under reduced pressure and the residue was purified by silica gel column chromatography (methylene chloride/methanol=10/1-5/1) to give 130 mg of t-butyl trans-(4-aminocyclohexyloxy)acetate as a colorless solid (57%).

1. temperatureby refluxing
2. temperatureunder heating for 2 hours
3. extractionextracted with benzene
4. washThe extract was washed with water and saturated brine
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationAfter filtration, low boiling matters
7. distillationwere distilled away from the filtrate under reduced pressure
8. customthe residue was purified by silica gel column chromatography (methylene chloride/methanol=10/1-5/1)