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1-(3-(Trifluoromethyl)phenyl)piperazine → 3-[4-(3-Trifluoromethylphenyl)-1-piperazinyl]propionic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-(3-(Trifluoromethyl)phenyl)piperazine | HCID 4296 | — |
| 反応物 | Ethyl 3-bromopropionate | HCID 68320 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-[4-(3-Trifluoromethylphenyl)-1-piperazinyl]propionic acid | HCID 11426605 | 75.2% |
反応手順
The reaction mixture of 1-(3-trifluoromethylphenyl)piperazine (510 mg, 2.2 mmol), ethyl 3-bromopropionate (500 mg, 2.7 mmol), sodium bicarbonate (300 mg, 3.5 mmol) and ethanol (15 ml) was refluxed for 3 h till the amine disappeared completely. After the mixture was filtered, the resulting solid was dissolved in 5 ml dioxane and 14 ml 5% sodium hydroxide solution. The mixture was stirred at room temperature overnight, then it was acidified with concentrated hydrogen chloride. Solid was filtered and washed with water, and then dried to give 500 mg 3-[4-(3-trifluoromethylphenyl)-1-piperazinyl]propionic acid as a white solid, mp 228-230° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06855720B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-789b1999ccb742508406e6b1f8486403 |
| 出典メモ | uspto-grants-2005_02 |