Sulfuric Acid → 2-Methoxy-3,5-heptanedione

온도

5 °C

In a 200 mL-volume flask equipped with a stirrer, a thermometer and a dropping funnel was placed 8.00 g (205 mmol) of sodium amide, and the flask was purged with argon. Then, 50 mL of toluene was placed in the flask. Subsequently, 15.0 g (208 mmol) of 2-butanone was slowly dropped into the ice-cooled mixture in the flask, and the resulting mixture was stirred for 10 minutes. The mixture was cooled to 5° C., and Into the cooled mixture was further dropped 8.50 g (72 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, 40 mL of water was placed in the flask under cooling with ice. The aqueous portion was taken out, made acetic with 2.5 mol/L sulfuric acid, and subjected to extraction with diethyl ether. The diethyl ether extract was washed with water, dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated and distilled under reduced pressure (32° C., 26.6 Pa) to give 5.60 g (yield: 49%) of 2-methoxy-3,5-heptanedione 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 diethyl ether
9. extractionThe diethyl ether 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 (32° C., 26.6 Pa)

ORD 기록

ord-374c4daf1315491ab6171decaa3ec319

출처 데이터셋

uspto-grants-2009_09

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07595414B2