참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 2-(2-Bromoethyl)-1,3-dioxolane | HCID 87776 | — |
| 반응물 | 5,6-Difluoropyridin-3-ol | HCID 68430860 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 5-[2-(1,3-Dioxolan-2-yl)ethoxy]-2,3-difluoropyridine | HCID 68429762 | 38.1% |
반응 단계
Cesium carbonate (33 g, 100 mmol) and 2-(2-bromoethyl)-1,3-dioxolane (12 g, 67 mmol) were added to an N,N-dimethylformamide suspension (30 ml) of 5,6-difluoropyridin-3-ol (8.8 g, 67 mmol), and stirred at 100° C. for 1 hour. The reaction solution was cooled to room temperature, water was added, and extracted with ethyl acetate. The organic layer was washed with saturated saline water, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane:chloroform=1:1 to 0:1) to obtain 5-[2-(1,3-dioxolan-2-yl)ethoxy]-2,3-difluoropyridine (5.9 g, yield: 38%) as a pale yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08846700B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-9e72d3e1c42543f1aabdb607ad88b529 |
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| 출처 메모 | uspto-grants-2014_09 |
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