Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → 3-Allyl-1,3-dimethyl-piperidin-4-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Allyl bromide | HCID 7841 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 1,3-Dimethyl-4-piperidone | HCID 107311 | — |
| 생성물 | 3-Allyl-1,3-dimethyl-piperidin-4-one | HCID 13740022 | — |
반응 단계
1,3-Dimethyl-piperidin-4-one (6 g, 47.24 mmol) was dissolved in 20 mL DMF and sodium hydride (2.07 g, 51.95 mmol) was added portionwise at 0° C. under nitrogen atmosphere. This was followed by dropwise addition of allyl bromide (5.71 g, 47.19 mmol) in 4 mL DMF at 0° C. under nitrogen atmosphere. The reaction mixture was stirred at RT for 15 min, quenched with ice-water and extracted with EtOAc (3×100 mL). The organic layer was washed with water (3×100 mL), dried over sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography (silica gel, 100-200 mesh) eluting with 7% EtOAc in hexane to obtain 3.2 g of 3-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-8092f642c0d046c0b72ce314b3e63012 |
| 출처 메모 | uspto-grants-2015_05 |