関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromoethene | HCID 11641 | — |
| 反応物 | I2-Ionone | HCID 638014 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1,4-Pentadien-3-ol, 3-methyl-1-(2,6,6-trimethyl-1-cyclohexen-1-yl)- | HCID 6436846 | 837.1% |
反応手順
0.1 mols of magnesium turnings are suspended in 50 ml of THF and treated with some drops of a solution of 0.12 mols of vinyl bromide in 100 ml of THF with stirring and under nitrogen atmosphere. As soon as the Grignard starts to form, the mixture is is cooled to 5-10° C. and added with the remaining solution of vinyl bromide in 30 min. The mixture is then cooled to −60° C. and added with 0.09 mols of beta ionone in 100 ml of THF in 20 min. The mixture is left to warm to room temperature, then heated at 40° C. for 2 hours. After that, the reaction is quenched as above described and vinyl beta-ionol is recovered by double distillation under vacuum, to obtain 166 g of a product, corresponding to an about 84% yield, with purity higher than 90%, determined by NMR.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06177579B1 |
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| 出典データセット | uspto-grants-2001_01 |
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| ORD ID | ord-209895f0c3fa4b99a666bb710cc5c737 |
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| 出典メモ | uspto-grants-2001_01 |
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