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1-{3-Methyl-5-[4-(trifluoromethyl)phenyl]thien-2-yl}ethanol → 1-[3-Methyl-5-(4-trifluoromethyl-phenyl)-thiophen-2-yl]-ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-{3-Methyl-5-[4-(trifluoromethyl)phenyl]thien-2-yl}ethanol | HCID 21986359 | — |
| 触媒 | Manganese dioxide | HCID 14801 | — |
| 生成物 | 1-[3-Methyl-5-(4-trifluoromethyl-phenyl)-thiophen-2-yl]-ethanone | HCID 57595000 | — |
反応手順
To a solution of 1-[3-Methyl-5-(4-trifluoromethyl-phenyl)-thiophen-2-yl]-ethanol (see Preparation 8) (4.40 g, 15.4 mmole), is added MnO2 (7.88 g, 77.0 mmole) in one portion. The mixture is heated under reflux for 16 hours, more MnO2 (7.88 g, 77.0 mmole) is added to the reaction and continued to reflux for 4 hours. The mixture is filtered through a celite pad, and the mother liquid is concentrated. The crude product is purified on a silica gel column, gradient eluting with 0-20% ethyl acetate in hexane and concentrated to provide the titled compound as yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07504433B2 |
| 出典データセット | uspto-grants-2009_03 |
| ORD ID | ord-256a6fe14b94461bbcd1ace5552bb17f |
| 出典メモ | uspto-grants-2009_03 |