Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2,4,6-Trifluorobenzoyl chloride → Benzamide, 2,4,6-trifluoro-N-(6-((1-methyl-4-piperidinyl)carbonyl)-2-pyridinyl)-, hydrochloride (1:1)
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2,4,6-Trifluorobenzoyl chloride | HCID 144895 | — |
| 반응물 | (6-Aminopyridin-2-yl)(1-methylpiperidin-4-yl)methanone | HCID 11401723 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | Benzamide, 2,4,6-trifluoro-N-(6-((1-methyl-4-piperidinyl)carbonyl)-2-pyridinyl)-, hydrochloride (1:1) | HCID 17980336 | 100% |
반응 단계
Combine 2-amino-6-(1-methylpiperidin-4-ylcarbonyl)pyridine (0.20 g, 0.92 mmol), 2,4,6-Trifluorobenzoyl chloride (0.357 g, 1.84 mmol), and 1,4-Dioxane (10 mL), and stir while heating at reflux. After 3 hr., cool the reaction mixture to ambient temperature and concentrate. Load the concentrated mixture onto an SCX column (10 g), wash with methanol, and elute with 2M ammonia in methanol. Concentrate the eluent to obtain the free base of the title compound as an oil (0.365 g (>100%)). Dissolve the oil in methanol (5 mL) and treat with ammonium chloride (0.05 g, 0.92 mmol). Concentrate the mixture and dry under vacuum to obtain the title compound. HRMS Obs. m/z 378.1435, Calc. m/z 378.1429; m.p. 255° C. (dec).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08748459B2 |
| 출처 데이터셋 | uspto-grants-2014_06 |
| ORD ID | ord-2a6312686e8842c5881fe80d6a74becd |
| 출처 메모 | uspto-grants-2014_06 |