関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 1-Phenyl-1,2-ethanediol | HCID 7149 | — |
| 反応物 | Paraldehyde | HCID 31264 | — |
| 触媒 | p-Toluenesulfonic acid | HCID 6101 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,3-Dioxolane, 2-methyl-4-phenyl- | HCID 118119 | 85.3% |
反応手順
100 g (0.63 mol) of (±)-1-phenyl-1,2-ethanediol (3) (87% pure according to GC) according to Example 1, 200 ml of toluene, 32 g (0.24 mol) of paraldehyde and 1 g of para-toluenesulfonic acid were charged to a 1 l stirrer, heated to boiling (110° C.) and stirred under reflux for a period of 4 h. A total of 10 ml of water were eliminated. After this time, the mixture was cooled to 20° C. and washed until neutral with sodium carbonate solution and water, and the solvent was distilled off under reduced pressure, leaving 103 g of crude product (85.3% pure according to GC). GC conditions see Example 2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07176176B2 |
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| 出典データセット | uspto-grants-2007_02 |
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| ORD ID | ord-794f4d0144e84dccaef656b3b1c84b40 |
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| 出典メモ | uspto-grants-2007_02 |
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