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1-Phenylpiperazine → 2-(4-Methyl-piperazin-1-yl)ethyl 4-phenylpiperazine-1-carboxylate formate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Phenylpiperazine | HCID 7096 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-(4-Methylpiperazin-1-yl)ethyl 4-nitrophenyl carbonate | HCID 57445007 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(4-Methyl-piperazin-1-yl)ethyl 4-phenylpiperazine-1-carboxylate formate | HCID 66650988 | 11.7% |
反応手順
2-(4-Methylpiperazin-1-yl)ethyl 4-nitrophenyl carbonate (Intermediate 4; 1.58 g, 5.1 mmol) was dissolved in DMF (25 mL). DIPEA (0.87 mL, 5.0 mmol) and 4-phenyl-piperazine (807 mg, 0.76 mL, 5.0 mmol) were added and the reaction mixture was stirred at room temperature for 14 hours. The reaction mixture was then concentrated in vacuo. The residue was purified by reverse phase column chromatography (gradient eluting with MeOH in water, with 1% formic acid in each solvent, 0-100%) to give 2-(4-methyl-piperazin-1-yl)ethyl 4-phenylpiperazine-1-carboxylate formate (113 mg, 6.7%) as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08093248B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-e3baaee6b1f2426fad3952ca369662ae |
| 出典メモ | uspto-grants-2012_01 |