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 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | alpha-Tocopherol | HCID 14985 | 100.2% |
反応手順
To a mixture consisting of 23.3 g (0.153 mol) of 2,3,5-trimethylhydroquinone, 17.5 g (0.128 mol) of zinc chloride, 54 ml of ethyl acetate and 2.5 g of concentrated hydrochloric acid, 46.1 g (0.153 mol) of isophytol (purity: 98.3%) was added dropwise under stirring at 25-30° over 3 hours. At the same temperature, the reaction mixture was stirred for an additional 2 hours. After the reaction mixture was washed with 10 ml of water, the solvent was distilled off. Toluene (100 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 66.0 g of the title compound was obtained as a brown oil (yield: 95.2%, GLC purity: 95.1%, α-tocopheryl acetate content: 2.0%, ethyl acetate recovery rate: 50%).
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-fdfc48f351b846e28cc3235c68551917 |
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| 出典メモ | uspto-grants-2000_02 |
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