関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 2-Bromopropane | HCID 6358 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Bromophenol | HCID 11563 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Bromo-3-isopropoxybenzene | HCID 3260801 | 89.8% |
反応手順
The following reagents were combined sequentially: anhydrous ethanol (880 ml), potassium carbonate (448.0 g), 3-bromophenol (386.7 g), 2-bromopropane (400.0 g) and finally water (88 ml). The mixture was heated at reflux (78° C.) for 16 hours. Water (880 ml) was added to the reaction mixture and 900 ml of solvent was removed by distillation at atmospheric pressure during a 4 hour period. Heptane (880 ml) was added to the reaction mixture and later separated. The aqueous layer was extracted with heptane (80 ml) and the combined organic fractions were washed sequentially with 1N HCl (300 ml), water (300 ml), 1N NaOH (300 ml) and water (300 ml). Removal of the solvent by rotary evaporation (50° C., 5 mmHg) afforded 453.6 g (97%) of crude product. This was distilled through a short path distillation column (81°-85° C., 2 mmHg) to provide 431.5 g of the product as a colorless liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05498718 |
|---|
| 出典データセット | uspto-grants-1996_03 |
|---|
| ORD ID | ord-16d25fc307704ba6a20526d0fa153864 |
|---|
| 出典メモ | uspto-grants-1996_03 |
|---|