化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Hydroxide → Bicyclo[4.2.0]octa-1,3,5,7-tetraen-7-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Tetrafluoroboric acid | HCID 28118 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 7-Bromobicyclo[4.2.0]octa-1,3,5-triene | HCID 568591 | — |
| 触媒 | Mercuric oxide | HCID 30856 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Bicyclo[4.2.0]octa-1,3,5,7-tetraen-7-ol | HCID 19963858 | — |
反応手順
To a stirred solution of mercury(II) oxide (591.3 mg, 2.73 mmol) and 35% aqueous tetrafluoroboric acid (TFBA) (999.4 mg, 5.46 mmol) in 1,4-dioxane (10.9 mL), 1-bromobenzocyclobutene (1.0 g, 5.46 mmol) was added. The reaction stirred at room temperature for 2 h and was then treated successively with NaHCO3 and 3N KOH until the solution remained basic. The precipitated mercury(II) oxide was filtered off and the filtrate extracted with CH2Cl2 (3×300 mL), dried with anhydrous Na2SO4, filtered, and concentrated to yield white crystals that were purified via column chromatography using a 3:2 Hexanes:EtOAc solvent system.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07935782B2 |
| 出典データセット | uspto-grants-2011_05 |
| ORD ID | ord-38950dbc02e44ffdad4df25a98661bc8 |
| 出典メモ | uspto-grants-2011_05 |