化工社化工社 化学情報印刷レポート · 研究参考用
Water → 6-Bromo-3,4-dimethoxybenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Veratraldehyde | HCID 8419 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 6-Bromo-3,4-dimethoxybenzaldehyde | HCID 79351 | 98% |
反応手順
To a solution of 500 g of 3,4-dimethoxybenzaldehyde in 2.5 L of methanol was added dropwise 529 g of bromine at room temperature (under cooling, if necessary) over 1 hour, and the mixture was stirred at the same temperature for 3 hours. To the reaction solution was added dropwise 2.5 L of water, and the crystals were precipitated. To the crystal suspension was added 20% aqueous sodium hydroxide solution at room temperature to adjust it to pH about 9 to 10, and then cooled. The precipitated crystals were collected by filtration and washed with water, and then dried at 50° C. for 12 hours to give 718.78 g of 6-bromo-3,4-dimethoxybenzaldehyde (yield: 98%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08754221B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-8abed474f4de4cbf94859ba33d902b02 |
| 出典メモ | uspto-grants-2014_06 |