Water → 2-Methoxy-6-methylheptane-3,5-dione

In a 200 mL-volume flask equipped with a stirrer, a thermometer and a dropping funnel was placed 5.15 g (132 mmol) of sodium amide, and the flask was purged with argon. Then, 80 mL of toluene was placed in the flask. Subsequently, 12.0 g (139.3-mmol) of 3-methyl-2-butanone was slowly dropped into the flask, and the resulting mixture was stirred for 15 minutes. Into the flask was further dropped 5.65 g (47.8 mmol) of methyl 2-methoxy-propionate (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, neutralized with acetic acid, and subjected to extraction with ether. The ether extract was washed with water, dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated and distilled under reduced pressure (41° C., 27 Pa) to give 4.25 g (yield: 52%) of 2-methoxy-6-methyl-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. customprepared by the method of Reference Example 1), and the mixture
4. stirringwas stirred for 30 minutes
5. customa reaction
6. temperatureunder cooling with ice
7. extractionsubjected to extraction with ether
8. extractionThe ether extract
9. washwas washed with water
10. dry with materialdried over anhydrous sodium sulfate
11. filtrationfiltered
12. concentrationThe filtrate was concentrated
13. distillationdistilled under reduced pressure (41° C., 27 Pa)

ORDレコード

ord-785c6ac33eb541139fcd78e4505f4979

出典データセット

uspto-grants-2009_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07595414B2