참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Chloromethyl Methyl Ether | HCID 7864 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 1-(6-Fluoropyridin-3-yl)ethan-1-ol | HCID 66600166 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Chloroform isopropyl alcohol | HCID 21906603 | — |
| 생성물 | 2-Fluoro-5-(1-methoxymethoxy-ethyl)-pyridine | HCID 66738292 | 66% |
반응 단계
Add N,N′-diisopropylethylamine and chloromethoxymethane to a solution of 1-(6-fluoro-pyridin-3-yl)-ethanol (3.0 g, 21.3 mmol) in dichloromethane at 0° C. Continue to stir the mixture for 30 min at 0° C., then overnight at room temperature. Dilute the mixture with chloroform/isopropyl alcohol (3/1). Wash the solution with saturated aqueous sodium chloride. Dry it over sodium sulfate. Concentrate the solution in vacuo to a dark residue. Purify by column chromatography (hexane→20% ethyl acetate in hexane) to afford the product as a colorless solid (3 g, 66%). MS (ES) m/z 186 [M+1]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08063212B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_11 |
|---|
| ORD ID | ord-fab50c36c9d14844a11c4da0c5f58bf0 |
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| 출처 메모 | uspto-grants-2011_11 |
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