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Salicyl Alcohol → [2-(2-Chlorobenzyloxy)phenyl]methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Salicyl Alcohol | HCID 5146 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | alpha-Bromo-o-chlorotoluene | HCID 11905 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | [2-(2-Chlorobenzyloxy)phenyl]methanol | HCID 961592 | 79.6% |
反応手順
A solution of 2.42 g (19.47 mmol) of 2-hydroxybenzyl alcohol in 100 ml of dry acetonitrile is mixed with 4.12 g (19.47 mmol) of 2-chlorobenzyl bromide and 2.96 g (21.42 mmol) of anhydrous potassium carbonate and heated to reflux for 12 hours. The mixture is then concentrated to dryness. The residue is taken up in ethyl acetate, washed with water and saturated sodium chloride solution and dried over sodium sulfate. The organic phase is concentrated. The resulting crude product is purified by flash chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 7:3). 3.856 g (15.5 mmol, 79% yield) of a solid are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07998988B2 |
| 出典データセット | uspto-grants-2011_08 |
| ORD ID | ord-8e3f0e4268514c848443ca63c3a9b4c0 |
| 出典メモ | uspto-grants-2011_08 |