化工社化工社 化学情報印刷レポート · 研究参考用
Ethylene Glycol → 4-(2-Methyl-1,3-dioxolan-2-yl)-2-nitrophenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | 4-Hydroxy-3-Nitroacetophenone | HCID 138723 | — |
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 4-(2-Methyl-1,3-dioxolan-2-yl)-2-nitrophenol | HCID 19026967 | — |
反応手順
A solution of 4'-hydroxy-3'-nitroacetophenone (known compound, 12.1 g, 67.0 mmol), benzene (100 ml), ethylene glycol (5.61 ml, 100 mmol) and p-toluenesulfonic acid hydrate (catalytic amount) was refluxed overnight removing the resulting water by azeotropic distillation with benzene. To the reaction mixture was added a saturated aqueous solution of sodium hydrogencarbonate, and the mixture was extracted with ethyl acetate, washed with saturated brine, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by column chromatography on silica gel to give the object compound (1) as an oil. Yield 14.6 g (97%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05308840 |
| 出典データセット | uspto-grants-1994_05 |
| ORD ID | ord-6c321d6e3ba54553a3cc0d0e00c56065 |
| 出典メモ | uspto-grants-1994_05 |