関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Pinacolone | HCID 6416 | — |
| 反応物 | Sodium amide | HCID 24533 | — |
| 反応物 | Propanoic acid, 2-methoxy-, methyl ester | HCID 86599 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Methoxy-6,6-dimethyl-3,5-heptanedione | HCID 24987127 | 52% |
反応手順
In a 200 mL-volume flask equipped with a stirrer, a thermometer and a dropping funnel was placed 8.20 g (210 mmol) of sodium amide, and the flask was purged with argon. Then, 80 mL of toluene was placed in the flask. Subsequently, 15.1 g (150.8 mmol) of 3,3-dimethyl-2-butanone was slowly dropped into the flask, and the resulting mixture was stirred for 15 minutes. Into the flask was further dropped 5.50 g (46.6 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, 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 (59° C., 492 Pa) to give 4.50 g (yield: 52%) of 2-methoxy-6,6-dimethyl-3,5-heptanedione as colorless liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07595414B2 |
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| 出典データセット | uspto-grants-2009_09 |
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| ORD ID | ord-28b2f7864fd24bfebc3c0dba4e1b25e9 |
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| 出典メモ | uspto-grants-2009_09 |
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