関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 2-Fluoro-5-formylpyridine | HCID 16414246 | — |
| 触媒 | Cupric chloride dihydrate | HCID 61482 | — |
| 溶媒 | Chloroform isopropyl alcohol | HCID 21906603 | — |
| 生成物 | 5-(1,3-Dioxolan-2-YL)-2-fluoropyridine | HCID 60155792 | 39% |
反応手順
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]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08063212B2 |
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| 出典データセット | uspto-grants-2011_11 |
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| ORD ID | ord-f668c9cefe1e479794ff2c53df520d50 |
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| 出典メモ | uspto-grants-2011_11 |
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