참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethylene Glycol | HCID 174 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | 2-Fluoro-5-formylpyridine | HCID 16414246 | — |
| 촉매 | Cupric chloride dihydrate | HCID 61482 | — |
| 용매 | Chloroform isopropyl alcohol | HCID 21906603 | — |
| 생성물 | 5-(1,3-Dioxolan-2-YL)-2-fluoropyridine | HCID 60155792 | 39% |
반응 단계
In a pressure vessel, combine 6-fluoro-pyridine-3-carbaldehyde (4 g, 32 mmol), ethylene glycol (3 g, 48 mmol), copper (II) chloride di-hydrate (0.56 g, 3.2 mmol) and THF (10 mL). Heat the mixture at 100° C. for 1 hour. Dilute the mixture with chloroform-isopropanol (3:1, 100 mL). Wash the organic phase with saturated aqueous sodium chloride and water. Dry the organic layer over sodium sulfate. Concentrate the solution in vacuo to brown oil. Purify by column chromatography (20% ethyl acetate in hexane) to afford the title compound (2.1 g, 39%) as a pale yellow oil. MS (ES) m/z 170 [M+1]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08063212B2 |
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| 출처 데이터셋 | uspto-grants-2011_11 |
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| ORD ID | ord-f668c9cefe1e479794ff2c53df520d50 |
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| 출처 메모 | uspto-grants-2011_11 |
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