Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3,5-Di-tert-butyl-4-hydroxybenzoic acid → 1-Benzyl-4-(3,5-di-t-butyl-4-hydroxy-benzoyl)piperazine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3,5-Di-tert-butyl-4-hydroxybenzoic acid | HCID 15007 | — |
| 반응물 | 1-Benzylpiperazine | HCID 75994 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-Benzyl-4-(3,5-di-t-butyl-4-hydroxy-benzoyl)piperazine | HCID 14300310 | — |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06706705B1 |
| 출처 데이터셋 | uspto-grants-2004_03 |
| ORD ID | ord-06a0725145a844dbb7713865c486204d |
| 출처 메모 | uspto-grants-2004_03 |