関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetaldehyde | HCID 177 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 1-Phenyl-1,2-ethanediol | HCID 7149 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,3-Dioxolane, 2-methyl-4-phenyl- | HCID 118119 | — |
反応手順
A 1 l stirrer fitted with reflux condenser, thermometer and dropping funnel was charged with 223 g (1.47 mol) of (±)-1-phenyl-1,2-ethanediol (3) (91% pure according to GC) from Example 1, 100 ml of diethyl ether and 2 g of para-toluenesulfonic acid and cooled to 5–10° C., and, at this temperature, 80.8 g (1.83 mol) of acetaldehyde were added over the course of 30 min. When the dropwise addition was complete, the mixture was then stirred firstly for 4 h at 5–10° C. and for a further 2 h at a maximum of 20° C. After this time, water was added, the organic phase was separated off, the aqueous phase was extracted with 1×100 ml of ether, and the combined organic phases were washed until neutral with sodium carbonate solution and water. Drying over Na2SO4 was then carried out, and the solvent was distilled off under reduced pressure.
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-4e8c8cddc40841dc9725bbbb58e46a5b |
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| 出典メモ | uspto-grants-2007_02 |
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