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3-Chloro-2-methylaniline → 1-(3-Chloro-2-methylphenyl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Chloro-2-methylaniline | HCID 6894 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Bis(2-chloroethyl)amine hydrochloride | HCID 522769 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | 1-(3-Chloro-2-methylphenyl)piperazine | HCID 3800845 | 81% |
反応手順
To a stirred solution of 3-chloro-2-methylaniline (21.6 g, 0.15 mol) in n-butanol (200 ml) was added bis(2-chloroethyl)amine hydrochloride (30 g, 0.17 mol) at room temperature and allowed to refluxed temperature for 2 days. After cooled to room temperature Na2CO3 (9 g, 0.08 mol) was added and then reaction mixture was refluxed 30 min. The resulting mixture was filtered with n-butanol (100 ml) and collected solid was dried under reduced pressure to be obtained title compound (24.8 g, 81%) as white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08895558B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-1cf06a9b55ae4c158ce1dc46b354b071 |
| 出典メモ | uspto-grants-2014_11 |