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Diethyl Ether → 1-{3-Methyl-5-[4-(trifluoromethyl)phenyl]thien-2-yl}ethanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 3-Methyl-5-[4-(trifluoromethyl)phenyl]thiophene-2-carbaldehyde | HCID 21986550 | — |
| 反応物 | HCID 178418689 | HCID 178418689 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-{3-Methyl-5-[4-(trifluoromethyl)phenyl]thien-2-yl}ethanol | HCID 21986359 | — |
反応手順
To a solution of 3-methyl-5-(4-Trifluoromethyl-phenyl)-thiophene-2-carbaldehyde (0.130 g, 0.481 mmole) in THF (5 mL), is injected 3.0 M MeMgBr in ethyl ether (0.27 mL, 0.810 mmole) dropwise. The reaction is stirred for 2 hours. The reaction is quenched with saturated NH4Cl(aq) (10 mL), then the aqueous solution is extracted with ethyl acetate (3×15 mL). The combined organic solution is washed with brine (3×50 mL), dried over Na2SO4 and concentrated. The crude product is purified on a silica gel column, 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-6c3090dad9ce47efa1756af0259d6d3c |
| 出典メモ | uspto-grants-2009_03 |