Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → trans-6-(2,5-Difluorophenyl)-1-benzyl-5-nitropiperidin-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Benzylamine | HCID 7504 | — |
| 반응물 | Methyl 4-nitrobutyrate | HCID 25604 | — |
| 반응물 | 2,5-Difluorobenzaldehyde | HCID 137663 | — |
| 반응물 | Sodium Acetate | HCID 517045 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | trans-6-(2,5-Difluorophenyl)-1-benzyl-5-nitropiperidin-2-one | HCID 67388890 | — |
반응 단계
To a solution of 2,5-difluorobenzaldehyde (1.09 g, 7.67 mmol) in ethanol (20 mL) were added methyl 4-nitrobutyrate (1.13 g, 7.04 mmol), benzylamine (0.98 mL, 7.67 mmol), sodium acetate (1.26 g, 15.3 mmol) and acetic acid (0.88 mL, 15.4 mmol). The mixture was stirred at rt for 12 h and then heated at reflux temperature overnight. After evaporation, the residue was purified by column chromatography (silica gel Biotage 40M™) eluting with ethyl acetate/hexane (gradient from 3% to 50%) to give the title compound as the racemic trans isomer. LC-MS: 347.1 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08653059B2 |
| 출처 데이터셋 | uspto-grants-2014_02 |
| ORD ID | ord-9c81f34126db454a9c58bf2b4af6f2ab |
| 출처 메모 | uspto-grants-2014_02 |