関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 5-Methyl-2-heptanone | HCID 28965 | — |
| 反応物 | HCID 178462451 | HCID 178462451 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Octyn-3-ol, 3,6-dimethyl- | HCID 174244 | 93% |
反応手順
128 g (1 mole) of 5-methyl-heptan-2-one are added in the course of 1 hour, with stirring, to 1 liter of a 1.1 molar solution of ethynyl-magnesium chloride in tetrahydrofuran at 10° C. After allowing about a further hour's reaction, the mixture is worked up. To do so, 2 N sulfuric acid is added, whilst cooling with ice, until two clear phases are present. The organic phase is then separated off and washed neutral with water, if necessary, and the tetrahydrofuran is distilled off at 50° C./67 mbar. The residue is subjected to fractional distillation. 143 g of main fraction, boiling at 50°-52° C./0.01 mbar, are obtained; nD25 =1.4411. This corresponds to a yield of 93%. Scent: predominantly floral, woody, herbal, minty with a spicy, slightly animal after-scent.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04347388 |
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| 出典データセット | uspto-grants-1982_08 |
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| ORD ID | ord-ec909e227fbe440faa5cc39a5bd828a5 |
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| 出典メモ | uspto-grants-1982_08 |
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