Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanesulfonyl chloride → Methanesulfonic acid 1-(6-fluoro-4-iodo-pyridin-3-yl)-ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanesulfonyl chloride | HCID 31297 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 1-(6-Fluoro-4-iodo-pyridin-3-yl)-ethanol | HCID 66738096 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Sodium Carbonate | HCID 10340 | — |
| 생성물 | Methanesulfonic acid 1-(6-fluoro-4-iodo-pyridin-3-yl)-ethyl ester | HCID 86641872 | 64.2% |
반응 단계
Add methanesulfonyl chloride (1.93 g, 16.8 mmol) to a solution of 1-(6-fluoro-4-iodo-pyridin-3-yl)-ethanol (1.5 g, 5.6 mmol) and diisopropylethylamine (2.2 g, 16.8 mmol) in DCM (50 mL) at 0° C. Continue to stir the mixture at 0° C. to RT for 4 h. Dilute the reaction mixture with diluted sodium carbonate. Extract the product into chloroform. Dry the organic phase over sodium sulfate. Concentrate the solution in vacuo. Purify the crude by column chromatography (20% ethyl acetate in hexane) to afford the title compound as a white solid (1.24 g, 64%). MS (ES) m/z 346 [M+1]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08114872B2 |
| 출처 데이터셋 | uspto-grants-2012_02 |
| ORD ID | ord-d9a872129cee474496a09887437bd7e9 |
| 출처 메모 | uspto-grants-2012_02 |