化工社化工社 化学情報印刷レポート · 研究参考用
Benzyl Bromide → 3'-hydroxy4'-benzyloxyacetophenone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzyl Bromide | HCID 7498 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3',4'-Dihydroxyacetophenone | HCID 14530 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 3'-hydroxy4'-benzyloxyacetophenone | HCID 10681628 | — |
反応手順
To a solution of 3′,4′-dihydroxyacetophenone (25.4 g) in N,N-dimethylacetamide (420 mL) were added potassium carbonate (23.1 g) and benzyl bromide (19.9 mL) under ice-cooling, and the mixture was stirred at room temperature for 90 minutes. An insoluble was filtered, and then diluted with ethyl acetate. The organic layer was sequentially washed with water and saturated saline, dried over magnesium sulfate, and then concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent: n-hexane→n-hexane/ethyl acetate=20/1), and then triturated with ethyl acetate to give 1-[4-(benzyloxy)-3-hydroxyphenyl]ethanone [REx(26-1)] (11.0 g) as a colorless powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09278944B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-b94a8c71df1443ab85c03bc52a6065f3 |
| 出典メモ | uspto-grants-2016_03 |