Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,2-Dichloroethane → N-methoxy-N-methyl-3-(pyridin-2-yl)propanamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,2-Dichloroethane | HCID 11 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 반응물 | 3-(Pyridin-2-yl)propanoic acid | HCID 564292 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | N-methoxy-N-methyl-3-(pyridin-2-yl)propanamide | HCID 78981096 | 79.3% |
반응 단계
A solution of 3-pyridin-2-yl-propionic acid (1.0 g, 6.62 mmol), DMAP (10 mg), and N,O-dimethylhydroxylamine hydrochloride (679 g, 7.0 mmol) and EDC (1.34 g, 7.0 mmol) in dichloromethane (40 mL) was treated with triethylamine (2.8 mL, 20.0 mmol). After stirring at room temperature overnight, the solution was poured into water, extracted with ethyl acetate (3×) and the combined organic phase was washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, filtered and concentrated. Purification by column chromatography (silica gel, 30-100% ethyl acetate in heptane) gave N-methoxy-N-methyl-3-(pyridin-2-yl)propanamide (1.02 g, 78%) as a colorless oil. ESI MS found for C10H14N2O2 m/z [195.1 (M+1)].
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09040703B2 |
| 출처 데이터셋 | uspto-grants-2015_05 |
| ORD ID | ord-6a376953aef548cfa575c005a815ef58 |
| 출처 메모 | uspto-grants-2015_05 |