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Water → 5-(3-Bromopropyl)-1,2,3-trimethoxybenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Phosphorus tribromide | HCID 24614 | — |
| 反応物 | 3-(3,4,5-Trimethoxyphenyl)Propan-1-Ol | HCID 6428843 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 5-(3-Bromopropyl)-1,2,3-trimethoxybenzene | HCID 22609611 | 84% |
反応手順
To a solution of 3-(3,4,5-trimethoxyphenyl)-propan-1-ol (9.50 g, 0.042 mol) in 50 ml of tetrahydrofuran, 5.0 ml (0.053 mol) of phosphorus tribromide were added dropwise at 0° C., followed by stirring at room temperature for 12 hours. The reaction mixture was added with water under ice cooling. The resulting solution was dissolved in 200 ml of ethyl acetate. The orqanic layer was washed successively with water, saturated NaHCO3 and saturated NaCl and then dried over anhydrous magnesium sulfate. The solvent was thereafter distilled off under reduced pressure. The oil thus obtained was purified by column chromatography (silica gel: "MERCK #9385", eluent: ether), whereby 10.2 g of the title compound were obtained as colorless oil (yield: 84%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05321135 |
| 出典データセット | uspto-grants-1994_06 |
| ORD ID | ord-3d1b16a97d0447d782c6317784bbae8a |
| 出典メモ | uspto-grants-1994_06 |