関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Acetaldehyde | HCID 177 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-(2,6,6-Trimethyl-3-cyclohexen-1-yl)-2-ethanone | HCID 21983366 | — |
| 溶媒 | Butyl Acetate | HCID 31272 | — |
| 生成物 | 1-(2,6,6-Trimethylcyclohex-3-en-1-yl)but-2-en-1-one | HCID 42296 | — |
反応手順
In a 250 ml flask were added 30 g (0.18 mole) of 1-(2,6,6-trimethyl-3-cyclohexen-1-yl)-2-ethanone (94% purity), 12.0 g of butyl acetate, an aliquot according to Table 1 of the catalytic solution as prepared above and a quantity of co-ingredient according to Table 1. The resulting mixture was stirred at 100° C. To said mixture, 4.0 g (0.09 mole) of acetaldehyde, diluted in 10 g of butyl acetate were introduced under the surface of the liquid, over 3 hours. After the completion of the introduction the reaction was cooled to 35° C. To the cooled reaction medium were added 10 g of acetic acid and then 40 ml of water. After stirring a few minutes, the water phase was removed and the organic phase was neutralized by washing it with 25 g of 20% aqueous potassium carbonate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091151B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-abb76655ac01447ea0ff9d306d69fe0b |
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| 出典メモ | uspto-grants-2006_08 |
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