反应详情

In a 200 mL-volume flask equipped with a stirrer, a thermometer and a dropping funnel was placed 10.1 g (259 mmol) of sodium amide, and the flask was purged with argon. Then, 120 mL of methylcyclohexane was placed in the flask. Subsequently, 7.40 g (127 mmol) of acetone was slowly dropped into the ice-cooled mixture in the flask, and the resulting mixture was stirred for 15 minutes. Into the flask was further dropped 15.0 g (127 mmol) of methyl 2-methoxypropionate (prepared by the method of Reference Example 1), and the mixture was stirred for 30 minutes for carrying out a reaction. After the reaction was complete, 50 mL of water was placed in the flask under cooling with ice. The aqueous portion was taken out, made acetic with acetic acid, and subjected to extraction with hexane. The hexane extract was washed with water, dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated and distilled under reduced pressure (66° C., 1.38 kPa) to give 9.63 g (yield: 53%) of 2-methoxy-3,5-hexanedione as colorless liquid.

1. customIn a 200 mL-volume flask equipped with a stirrer
2. customthe flask was purged with argon
3. temperaturecooled mixture in the flask
4. customprepared by the method of Reference Example 1), and the mixture
5. stirringwas stirred for 30 minutes
6. customa reaction
7. temperatureunder cooling with ice
8. extractionsubjected to extraction with hexane
9. extractionThe hexane extract
10. washwas washed with water
11. dry with materialdried over anhydrous sodium sulfate
12. filtrationfiltered
13. concentrationThe filtrate was concentrated
14. distillationdistilled under reduced pressure (66° C., 1.38 kPa)