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Methyl Salicylate → Methyl 2-(3-iodopropoxy)-benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl Salicylate | HCID 4133 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 1,3-Diiodopropane | HCID 12314 | — |
| 反応物 | Ethyl acetate hexane | HCID 21226206 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | Methyl 2-(3-iodopropoxy)-benzoate | HCID 18333395 | — |
反応手順
Combine methyl salicylate (5.09 g, 33.2 mmol), sodium carbonate (10.56 g, 99.67 mmol), and 1,3-diiodopropane (29.49 g, 99.67 mmol) in acetone (200 mL). Heat to reflux. After 18 hours, add sodium carbonate (10.56 g, 99.67 mmol) and continue to heat at reflux. After 18 hours, add 1,3-diiodopropane (29.49 g, 99.67 mmol) and continue to heat at reflux. After 18 hours. filter the reaction mixture and concentrate the filtrate in vacuo to give a residue. Chromatograph the residue on silica gel eluting with 1/10 ethyl acetate/hexane to give the title compound: Rf=0.29 (silica gel, 1/10 ethyl acetate/hexane).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06329392B1 |
| 出典データセット | uspto-grants-2001_12 |
| ORD ID | ord-f75a37c539eb41af931f147e96adde1a |
| 出典メモ | uspto-grants-2001_12 |