化工社化工社 化学情報印刷レポート · 研究参考用
3,5-Di-tert-butyl-4-hydroxybenzoic acid → 1-Benzyl-4-(3,5-di-t-butyl-4-hydroxy-benzoyl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3,5-Di-tert-butyl-4-hydroxybenzoic acid | HCID 15007 | — |
| 反応物 | 1-Benzylpiperazine | HCID 75994 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-Benzyl-4-(3,5-di-t-butyl-4-hydroxy-benzoyl)piperazine | HCID 14300310 | — |
反応手順
Under nitrogen atmosphere, 3,5-di-t-butyl-4-hydroxy-benzoic acid (3.10 g, 12.4 mmol.) and 1-benzylpiperazine (2.00 g, 11.3 mmol.) were dissolved in dichloromethane. Under chilling with ice, to this solution was portionwise added 1-(3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride (2.87 g, 15.0 mmol.), and the resulting mixture was stirred overnight at room temperature. The reaction mixture was washed successively with saturated aqueous sodium hydrogen carbonate and water, and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (chloroform/methanol=20/1), to give the desired compound as an amorphous product (5.08 g, yield: 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06706705B1 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-06a0725145a844dbb7713865c486204d |
| 出典メモ | uspto-grants-2004_03 |