関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Mepp | HCID 91965 | — |
| 反応物 | 2-(2,4-Dimethoxyphenyl)acetic acid | HCID 350555 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(2,4-Dimethoxyphenylacetyl)-4-(2-methylphenyl)piperazine | HCID 8297091 | — |
反応手順
1-(2-methylphenyl)piperazine (.087 g, 0.41 mmol) and 2,4-dimethoxyphenylacetic acid (0.096 g, 0.49 mmol) were dissolved in 20 DMF (5 ml) and treated with EDC (0.091 g, 0.47 mmol) and HBT (0.071 g, 0.52 mmol). Triethylamine was added to the stirred mixture to bring the pH (moistened E. Merck colorpHast indicator) to ca. 9. The mixture was stirred at ambient temperature for 18 hours, then concentrated in vacuo. The residue was taken up in ethyl acetate, and the ethyl acetate layer was washed with saturated aqueous sodium bicarbonate and brine, dried over sodium sulfate, filtered, and the filtrate was concentrated to dryness in vacuo. The residue was chromatographed on silica gel eluted with 1.5% methanol in methylene chloride. The combined product fractions were evaporated to dryness in vacuo to give the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05756504 |
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| 出典データセット | uspto-grants-1998_05 |
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| ORD ID | ord-6c0f53a3127d4a04baf5e948c80f9ef1 |
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| 出典メモ | uspto-grants-1998_05 |
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