Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3-Chloro-4-(trifluoromethyl)aniline → N-[3-chloro-4-(trifluoromethyl)phenyl]-4-[(1-methylpiperidin-3-yl)methyl]piperazine-1-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3-Chloro-4-(trifluoromethyl)aniline | HCID 67962 | — |
| 반응물 | Di-tert-butyl dicarbonate | HCID 90495 | — |
| 반응물 | 1-[(1-Methylpiperidin-3-yl)methyl]piperazine | HCID 2736940 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | N-[3-chloro-4-(trifluoromethyl)phenyl]-4-[(1-methylpiperidin-3-yl)methyl]piperazine-1-carboxamide | HCID 11596912 | 6.7% |
반응 단계
To a solution of di-tert-butyl dicarbonate (114.6 mg) in chloroform (2 ml) was added 4-dimethylaminopyridine (6 mg). A solution of 4-amino-2-chlorobenzotrifluoride (98.1 mg) in chloroform (2 ml) was added and the reaction mixture stirred for 20 minutes at room temperature. A solution of 1-[(1-methylpiperidin-3-yl)methyl]piperazine (98.5 mg) in chloroform (2 ml) was added and the resulting solution was stirred at reflux for 18 hours. The reaction mixture was purified by column chromatography on silica gel (20 g) using a gradient of 100% dichloromethane through to 20% methanolic ammonia in dichloromethane to give the title compound (14 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07906645B2 |
| 출처 데이터셋 | uspto-grants-2011_03 |
| ORD ID | ord-756c6bebf35b4f39a1dcfd943e37587b |
| 출처 메모 | uspto-grants-2011_03 |