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Pyridine → 3-(2-Ethoxyphenoxy)-1,2-propanediol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Glycidol | HCID 11164 | — |
| 反応物 | 2-Ethoxyphenol | HCID 66755 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-(2-Ethoxyphenoxy)-1,2-propanediol | HCID 68825 | 65.6% |
反応手順
A solution of 41.5 g (0.3 mole) of 2-ethoxyphenol, 29.6 g (0.4 mole) of glycidol, 2 ml of pyridine and 150 ml of absolute ethanol was heated at reflux temperature for 18 hr. The mixture was concentrated to a thick oil that crystallized slowly over several days. The crude product was chromatographed on a silica gel column (1.2 kg) using increasing portions of acetone in methylene chloride to elute the product. The desired fractions were combined and concentrated to give a yellow oil that crystallized on standing. The solid was triturated with petroleum ether and the mixture filtered to obtain 41.8 g of solid. Recrystallization from carbon tetrachloride yielded 37.2 g (58%) of white solid, mp 64°-65° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05273993 |
| 出典データセット | uspto-grants-1993_12 |
| ORD ID | ord-c53d4bf680f5421caf8433d94405f16d |
| 出典メモ | uspto-grants-1993_12 |