Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 1-(1-Methylpiperidin-4-yl)-4-((1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-2-yl)methylsulfonyl)piperazine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1-(1-Methyl-4-piperidinyl)piperazine | HCID 566324 | — |
| 반응물 | (1-(3-(Trifluoromethyl)phenylsulfonyl)piperidin-2-yl)methanesulfonyl chloride | HCID 59367748 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-(1-Methylpiperidin-4-yl)-4-((1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-2-yl)methylsulfonyl)piperazine | HCID 46204976 | 30% |
반응 단계
1-(1-Methyl-4-piperidinyl)piperazine (1.126 mmol) was dissolved in methylene chloride (7 ml), the solution was cooled in an ice bath and triethylamine (2.8 mmol) and (1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-2-yl)methanesulfonic acid chloride (dissolved in methylene chloride (3 ml)) were added. The mixture was stirred for 16 h, during which it was allowed to warm slowly to room temperature. The reaction mixture was diluted with methylene chloride and washed with water and the organic phase was dried over sodium sulfate and concentrated in vacuo. The crude product was purified by column chromatography (silica gel) with methylene chloride/methanol (19:1). Yield: 30%. MS, Rt=2.4 min, m/z=553.0 [MH]+
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08119805B2 |
| 출처 데이터셋 | uspto-grants-2012_02 |
| ORD ID | ord-64b94bdc6da8478e9d722c226b99b3b0 |
| 출처 메모 | uspto-grants-2012_02 |