反应详情

温度

80 °C

To a solution of the obtained 2-methyl-2-propanyl (3R)-3-{[(4-hydroxy-2-methyl-5-nitrophenyl)carbonyl](2-propanyl)amino}-1-piperidinecarboxylate (138 g) in N,N-dimethylformamide (1000 ml) were added potassium carbonate (91 g), diethyl 2-bromo-2-methylmalonate (94 g), and the mixture was stirred at 80° C. for 8 hours. The reaction solution was allowed to cool to room temperature, filtered through celite, and to the filtrate were added a 5% aqueous sodium hydrogen sulfate solution and ethyl acetate, and extracted with ethyl acetate. The organic layer was washed with water, a saturated aqueous sodium chloride solution, and then dried over sodium sulfate. The sodium sulfate was removed by filtration, and the filtrate was concentrated under reduced pressure to give diethyl methyl(5-methyl-4-{[(3R)-1-{[(2-methyl-2-propanyl)oxy]carbonyl}-3-piperidinyl](2-propanyl)carbamoyl}-2-nitrophenoxy)propanedioate (205 g).

1. temperatureto cool to room temperature
2. filtrationfiltered through celite
3. additionto the filtrate were added a 5% aqueous sodium hydrogen sulfate solution and ethyl acetate
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with water
6. dry with materiala saturated aqueous sodium chloride solution, and then dried over sodium sulfate
7. customThe sodium sulfate was removed by filtration
8. concentrationthe filtrate was concentrated under reduced pressure