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1,2-Dichloroethane → 1-(2,4-Dimethoxyphenylacetyl)-4-(2-methylphenyl)piperazine-2-carboxamide
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-(2,4-Dimethoxyphenyl)acetic acid | HCID 350555 | — |
| 反応物 | 2-Carbamoyl-4-(2-methylphenyl)piperazine | HCID 15430568 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(2,4-Dimethoxyphenylacetyl)-4-(2-methylphenyl)piperazine-2-carboxamide | HCID 18914149 | — |
反応手順
4-(2-Methylphenyl)piperazine-2-carboxamide (39 mg, 0.18 mmol), 2,4-dimethoxyphenylacetic acid (42 mg, 0.21 mmol), EDC (42 mg, 0.22 mmol) and HBT (31 mg, 0.23 mmol) were combined in DMF (5 ml) and treated with triethylamine to adjust the pH to ca. 9 (moistened E. Merck colorpHast indicator). The mixture was stirred at ambient temperature for 64 hours. The solvent was removed in vacuo and the residue was chromatographed on silica gel eluted with 2% methanol in methylene chloride. The combined product fractions were evaporated to dryness in vacuo to provide the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05756504 |
| 出典データセット | uspto-grants-1998_05 |
| ORD ID | ord-e7ca6f9b6cb74790b78a4231cd52599c |
| 出典メモ | uspto-grants-1998_05 |