関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,4-Benzodioxan | HCID 10301 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | 2-Bromo-5-iodobenzoyl chloride | HCID 58340809 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methanone, (2-bromo-5-iodophenyl)(2,3-dihydro-1,4-benzodioxin-6-yl)- | HCID 58340798 | 88.4% |
反応手順
To a stirred solution of 2-bromo-5-iodo-benzoyl chloride (26.4 g, 76.56 mmol) in dichloromethane (250 mL) was added benzo(1,4)-dioxane (10.41 g, 76.26 mmol) at 0° C. To this reaction mixture, AlCl3 (40.78 g, 305.47 mmol) was added in portions. After stirring overnight at room temperature, the reaction mixture was poured into crushed ice. The resulting mixture was extracted with dichloromethane (500 mL×2). The dichloromethane layers were combined and washed with water (200 mL), saturated aqueous sodium bicarbonate solution (200 mL×2), and brine (200 mL), then dried over sodium sulfate and concentrated. The solid product was triturated with hexanes, and the triturated product was dried under vacuum to furnish (2-bromo-5-iodo-phenyl)-(2,3-dihydro-benzo[1,4]dioxin-6-yl)-methanone (30 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08466114B2 |
|---|
| 出典データセット | uspto-grants-2013_06 |
|---|
| ORD ID | ord-bf29f2e62f324d66bd4cf2029aafc6d2 |
|---|
| 出典メモ | uspto-grants-2013_06 |
|---|