関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | Methyl acetoacetate | HCID 7757 | — |
| 反応物 | 2-Methyl-3-butyn-2-ol | HCID 8258 | — |
| 触媒 | Aluminum tri(methyl acetylacetate) | HCID 18676716 | — |
| 溶媒 | Propylene Carbonate | HCID 7924 | — |
| 生成物 | 6-Methylhepta-3,5-dien-2-one | HCID 27971 | 72% |
反応手順
A mixture of 5.3 g of the aluminum tri(methyl acetylacetate) catalyst mentioned in Example 1 and 85 g of 1,2-propylene carbonate was heated to 170° C. and, at this temperature a mixture of 55 g (0.47 mol) of methyl acetoacetate and 43.7 g (0.52 mol) of 2-methyl-3-butyn-2-ol was metered in at a constant rate over the course of 4 h. After the addition was complete, the mixture was stirred at 170° C. for 30 min. During this time, CO2 was evolved and low boilers distilled out. The reaction mixture was subsequently cooled, and the 2-methyl-2,4-heptadien-6-one which was formed was distilled out under about 100 mbar. This resulted in 42 g of pure 2-methyl-2,4-heptadien-6-one, which corresponds to a yield of 72% of theory based on reacted 2-methyl-3-butyn-2-ol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05874635 |
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| 出典データセット | uspto-grants-1999_02 |
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| ORD ID | ord-4457941ebbf8475a829019b2152c533d |
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| 出典メモ | uspto-grants-1999_02 |
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