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Trichloroacetic Acid → 2,2,2-Trichloro-1-(4-(4-methylpiperazine-1-yl)phenyl)ethanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trichloroacetic Acid | HCID 6421 | — |
| 反応物 | 4-(4-Methylpiperazin-1-yl)benzaldehyde | HCID 736533 | — |
| 反応物 | Sodium Trichloroacetate | HCID 23681045 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2,2,2-Trichloro-1-(4-(4-methylpiperazine-1-yl)phenyl)ethanol | HCID 68277172 | 82% |
反応手順
1.0 ml (10.00 mmol) of trichloroacetic acid and, in small portions, 1.854 g. (10 mmol) of sodium 2,2,2-trichloroacetate are added at room temperature to a solution of 1.362 g (6.67 mmol) of 4-(4-methylpiperazine-1-yl)benzaldehyde in 13.5 ml of dimethylformamide. The reaction mixture is stirred for 3 hours at room temperature. The solvent is concentrated and the crude reaction product extracted with ethyl acetate. The organic phase is washed using saturated sodium bicarbonate solution. The organic phases are combined, dried on magnesium sulfate and then concentrated to yield 1.760 g (yield=82%) of 2,2,2-trichloro-1-(4-(4-methylpiperazine-1-yl)phenyl)ethanol in the form of a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08883821B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-515ca87369a043708f8648e14abc16e2 |
| 出典メモ | uspto-grants-2014_11 |