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Methyl Salicylate → Methyl 2-(2-chloroethoxy)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl Salicylate | HCID 4133 | — |
| 反応物 | 1-Bromo-2-Chloroethane | HCID 7849 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 生成物 | Methyl 2-(2-chloroethoxy)benzoate | HCID 9837283 | — |
反応手順
34 g (0.25 mol) of potassium carbonate were added to a solution of 25 g (0.16 mol) of methyl salicylate in 250 ml of methyl ethyl ketone. This mixture was refluxed for 1 h, then 27.3 ml (0.35 mol) of 1-bromo-2-chloro-ethane were added and the mixture was taken to reflux again. Four hours later, 34 g (0.25 mol) more of potassium carbonate and 16.3 ml (0.2 mol) more of 1-bromo-2-chloro-ethane were added. This operation was repeated until the reaction was completed. The inorganic salts were filtered off and the liquid phase was diluted with the same volume of hexane. This organic phase was washed twice with water and worked-up as usual. The yield in this step was quantitative and the product was pure enough for the next synthetic step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07189741B2 |
| 出典データセット | uspto-grants-2007_03 |
| ORD ID | ord-9aabaa3017474a3ca3687eecadcc13ca |
| 出典メモ | uspto-grants-2007_03 |