化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → Ethyl 3-methoxy-4-[[(trifluoromethyl)sulfonyl]oxy]benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Ethyl vanillate | HCID 12038 | — |
| 反応物 | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ethyl 3-methoxy-4-[[(trifluoromethyl)sulfonyl]oxy]benzoate | HCID 22171362 | — |
反応手順
Trifluoromethanesulfonic anhydride (0.94 mL) was added to an ice-cooled mixture of ethyl vanillate (1.0 g) and pyridine (0.45 mL) in methylene chloride (5 mL) with stirring. The mixture was stirred for 10 min, and poured into a mixture of 1 mol/L hydrochloric acid and ethyl acetate. The organic layer was separated, washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (eluent:ethyl acetate/n-hexane=1/10) to afford ethyl 3-methoxy-4-trifluoromethanesulfonyloxybenzoate (1.47 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07423185B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-178c977206fe4786a5e3c897eb1be400 |
| 出典メモ | uspto-grants-2008_09 |