Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2-(Dimethylamino)ethanol → (6-Chloropyridin-2-yl)(1-methylpiperidin-4-yl)methanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2-(Dimethylamino)ethanol | HCID 7902 | — |
| 반응물 | 2-Chloropyridine | HCID 7977 | — |
| 반응물 | N-Methoxy-N,1-dimethylpiperidine-4-carboxamide | HCID 23499459 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | (6-Chloropyridin-2-yl)(1-methylpiperidin-4-yl)methanone | HCID 10705139 | 47.6% |
반응 단계
Add 2-chloropyridine (1 g, 8.8 mmole) to a mixture of n-butyl lithium (1.6 M in hexane) (22 mL, 35.2 mmole) and 2-dimethylamino-ethanol (1.56 g, 17.6 mmole) in hexane (20 mL at −78° C.) and stirred for 1 hour. Then add 1-methyl-piperidine-4-carboxylic acid methoxy-methyl-amide (3.2 g, 17.6 mmole) in hexane (5 mL) and stir the mixture for 1 hour. Quench the reaction mixture with water and extract twice with ethyl acetate, dry the organic layer with anhydrous sodium sulfate, evaporate the solvent and purify the residual product by chromatography on a silica gel column to give about 1 g of the title product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08044207B2 |
| 출처 데이터셋 | uspto-grants-2011_10 |
| ORD ID | ord-ebf4b78743b7428dbdd81a8422e679a6 |
| 출처 메모 | uspto-grants-2011_10 |