反应详情

温度

70 °C

A mixture of ethyl 4-(4-amino-2-methoxycarbonylphenoxy)butyrate (2.20 g), bis(2-chloroethyl)ether (0.915 ml, 7.81 mmol), potassiumcarbonate(3.24 g, 23.4 mmol), sodium iodide (2.34 g, 15.6 mmol) and DMF (20 ml) was stirred at 70° C. for 24 hours, and the mixture was concentrated under reduced pressure. To the residue was added water, and the mixture was extracted with ethyl acetate. The organic layer was dried with anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified with column chromatography (silica gel 30 g, ethyl acetate/hexane=1/4), and the desired fraction was concentrated under reduced pressure to give ethyl 4-(2-methoxycarbonyl-4-morpholinophenoxy)butyrate (2.18 g).

1. concentrationthe mixture was concentrated under reduced pressure
2. additionTo the residue was added water
3. extractionthe mixture was extracted with ethyl acetate
4. dry with materialThe organic layer was dried with anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified with column chromatography (silica gel 30 g, ethyl acetate/hexane=1/4)
7. concentrationthe desired fraction was concentrated under reduced pressure