Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methylamine → trans-6-(2,5-Difluorophenyl)-1-methyl-5-nitropiperidin-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | Methyl 4-nitrobutyrate | HCID 25604 | — |
| 반응물 | 2,5-Difluorobenzaldehyde | HCID 137663 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | trans-6-(2,5-Difluorophenyl)-1-methyl-5-nitropiperidin-2-one | HCID 67389784 | — |
반응 단계
To a solution of 2,5-difluorobenzaldehyde (0.765 mL, 7.04 mmol) in ethanol (15 mL) were added methyl 4-nitrobutyrate (0.901 mL, 7.04 mmol) and methylamine (7.04 mL, 14.07 mmol). The mixture was 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 40% to 60%) to give the title compound as the racemic trans isomer. LC-MS: 271.05 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08653059B2 |
| 출처 데이터셋 | uspto-grants-2014_02 |
| ORD ID | ord-1e31ca7127cd4dd08659570443fd9ba5 |
| 출처 메모 | uspto-grants-2014_02 |