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Triethylamine → 1-Methyl-3-phenyl-4-(4-chlorophenacyl) piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | p-Chlorophenacyl bromide | HCID 68303 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1-Methyl-3-phenylpiperazine | HCID 2760009 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Methyl-3-phenyl-4-(4-chlorophenacyl) piperazine | HCID 14302344 | 95% |
反応手順
To a stirred mixture of 14.0 g (0.08 mol) of 1-methyl-3-phenylpiperazine and 20 g (0.2 mol) of triethylamine in 160 ml of tetrahydrofuran was added dropwise a solution of 18.2 g (0.08 mol) of 4-chlorophenacyl bromide in 55 ml of chloroform. The resulting mixture was stirred at ambient temperature for 3.5 hours, poured into 50% aqueous sodium bicarbonate and extracted with chloroform. The organic extracts were combined, washed with water and saturated sodium chloride and dried over sodium sulfate. The filtrate was concentrated to dryness to give 25 g of crude 1-methyl-3-phenyl-4-(4-chlorophenacyl) piperazine. This material was used as such in the next step of the process.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04772705 |
| 出典データセット | uspto-grants-1988_09 |
| ORD ID | ord-8f0182d5fffe48fb93eae2b4751f2601 |
| 出典メモ | uspto-grants-1988_09 |