化工社化工社 化学情報印刷レポート · 研究参考用
Ethylene Glycol → 1-Bromo-3-(1,3-dioxolan-2-YL)-4-methoxybenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | 5-Bromo-2-methoxybenzaldehyde | HCID 90684 | — |
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-Bromo-3-(1,3-dioxolan-2-YL)-4-methoxybenzene | HCID 22349589 | 62.3% |
反応手順
To a stirred solution of 5-bromo-2-methoxybenzaldehyde (5.0 g, 23.25 mmol) in toluene (50 mL) was added ethylene glycol (2.6 mL, 46.5 mmol) and p-toluenesulfonic acid monohydrate (0.45 g, 2.32 mmol) and the reaction mixture was azeotroped for 2 h, quenched with sat. NaHCO3 (50 mL). Reaction mixture was concentrated under reduced pressure, extracted with ethyl acetate (2×100 mL), washed with water, brine, dried over sodium sulfate, concentrated and purified by silica gel column chromatography to furnish 2-(5-bromo-2-methoxy-phenyl)-[1,3]dioxolane (3.75 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08828951B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-107b1be43fc44a18b54e16138cfe2a3a |
| 出典メモ | uspto-grants-2014_09 |