関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Isophytol | HCID 10453 | — |
| 反応物 | Trimethylhydroquinone | HCID 12785 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 溶媒 | Isobutyl Acetate | HCID 8038 | — |
| 生成物 | alpha-Tocopherol | HCID 14985 | 102.2% |
反応手順
To a mixture consisting of 69.9 g (0.460 mol) of 2,3,5-trimethylhydroquinone, 52.5 g (0.386 mol) of zinc chloride, 150 ml of isobutyl acetate and 7.5 g of concentrated hydrochloric acid, 138.3 g (0.459 mol) of isophytol (purity: 98.3%) was added dropwise under stirring at 30-40° C. over 3 hours. At the same temperature, the reaction mixture was stirred for an additional 2 hours. After the reaction mixture was washed with 30 ml of water, the solvent was distilled off. Toluene (300 ml) was added to the residue to dissolve the same. The resulting solution was washed successively with water, alkaline water and a saturated aqueous solution of NaCl, dried over magnesium sulfate and then concentrated under reduced pressure, whereby 202.0 g of the title compound was obtained as a brown oil (yield 99.6%, GLC purity: 97.5).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06020505 |
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| 出典データセット | uspto-grants-2000_02 |
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| ORD ID | ord-5fe197cbf00d42d2bf19274f6e311a6a |
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| 出典メモ | uspto-grants-2000_02 |
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