Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diisopropylethylamine → 3,4-Dichlorophenyl 4-[(1-methylpiperidin-3-yl)methyl]piperazine-1-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 1-[(1-Methylpiperidin-3-yl)methyl]piperazine | HCID 2736940 | — |
| 반응물 | 3,4-Dichlorophenyl carbonochloridate | HCID 13077890 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3,4-Dichlorophenyl 4-[(1-methylpiperidin-3-yl)methyl]piperazine-1-carboxylate | HCID 57656732 | 60.6% |
반응 단계
3,4-Dichlorophenyl chloroformate (282 mg) in dichloromethane (10 ml) was added to a solution of 1-[(1-methylpiperidin-3-yl)methyl]piperazine (246 mg) in dichloromethane (2 ml) at room temperature. N,N-Diisopropylethylamine (0.44 ml) was added and the mixture stirred for 18 hours. Saturated aqueous sodium bicarbonate solution (5 ml) was added and the dichloromethane layer separated then concentrated in vacuo onto silica gel (0.5 g). The resulting powder was subjected to chromatography on silica gel (20 g) using a gradient of 100% dichloromethane through to 20% methanolic ammonia in dichloromethane to give the title compound (292 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08710224B2 |
| 출처 데이터셋 | uspto-grants-2014_04 |
| ORD ID | ord-65f958bc4af24553b7b772b49832bf1f |
| 출처 메모 | uspto-grants-2014_04 |