Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → 3-[2-(4-Fluoro-phenyl)-allyl]-1,3-dimethyl-piperidin-4-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 1,3-Dimethyl-4-piperidone | HCID 107311 | — |
| 반응물 | 1-(3-Bromoprop-1-en-2-yl)-4-fluorobenzene | HCID 11694212 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-[2-(4-Fluoro-phenyl)-allyl]-1,3-dimethyl-piperidin-4-one | HCID 67355960 | 52.1% |
반응 단계
To a stirred solution of 1,3-dimethylpiperidin-4-one (2.8 g, 22.04 mmol) in DMF (10 mL) was added sodium hydride (970 mg, 24.25 mmol) at 0° C. After stiffing for 5 min, 1-(1-bromomethyl-vinyl)-4-fluoro-benzene (4.74 g, 22.04 mmol) was added dropwise and stirring was continued for 30 min. The reaction was quenched with ice water and extracted with EtOAc (2×100 mL). The combined organic layer was washed with water (4×100 mL), dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography using silica (100:200) and 10% EtOAc-Hex as eluent to yield 3 g of 3-[2-(4-fluoro-phenyl)-allyl]-1,3-dimethyl-piperidin-4-one.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09040519B2 |
| 출처 데이터셋 | uspto-grants-2015_05 |
| ORD ID | ord-3ca1e346b67140bbace1cd181e882fd3 |
| 출처 메모 | uspto-grants-2015_05 |