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Potassium Carbonate → 1-Methyl-4-(3-nitrobenzyl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | alpha-Chloro-m-nitrotoluene | HCID 12078 | — |
| 反応物 | 1-Methylpiperazine | HCID 53167 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 1-Methyl-4-(3-nitrobenzyl)piperazine | HCID 1377109 | — |
反応手順
A mixture of 3-nitrobenzylchloride (5 g, 29.14 mmol), N-methylpiperazine (3.9 mL, 34.97 mmol, 1.2 equiv), potassium carbonate (8 g, 58.28, 2 equiv), and acetone (100 ml) is stirred for 15 h at reflux. The reaction mixture is allowed to cool to RT, filtered and concentrated. The residue is purified by silica gel MPLC (DCM/MeOH+1% NH3aq, 95:5) to afford the title compound as a brow oil: ESI-MS: 236.0 [MH]+; tR=1.40 min (purity: 100%, system 1); TLC: Rf=0.31 (DCM/MeOH+1% NH3aq, 9:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08759517B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-7d1ba0dbc3484685a2a900127b7440b4 |
| 出典メモ | uspto-grants-2014_06 |