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4-Toluenesulfonyl chloride → 1-Acetyl-4-(2-chloroethyl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Acetyl-4-(2-hydroxyethyl)piperazine | HCID 4739629 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-Acetyl-4-(2-chloroethyl)piperazine | HCID 13289488 | 54.3% |
反応手順
2-(4-Acetylpiperazin-1-yl)ethanol (500 mg, 2.90 mmol), (prepared as described for the starting material in this example hereinbefore), was dissolved in methylene chloride (10 ml) and triethylamine (445 μl, 3.19 mmol) and 4-toluenesulphonyl chloride (609 mg, 3.19 mmol) were added and the mixture was stirred at ambient temperature overnight. The mixture was washed with brine, dried (MgSO4) and concentrated under reduced pressure. The residue was purified by column chromatography eluting with methylene chloride/methanol (98/2) to give 1-acetyl-4-(2-chloroethyl)piperazine (300 mg, 54%) as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07268230B2 |
| 出典データセット | uspto-grants-2007_09 |
| ORD ID | ord-2f4d03f2efd1421885b5b5b054254a73 |
| 出典メモ | uspto-grants-2007_09 |