関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | 2-(2-Bromoethyl)-1,3-dioxolane | HCID 87776 | — |
| 反応物 | 6-Fluoropyridin-3-ol | HCID 2763108 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 5-[2-(1,3-Dioxolan-2-yl)ethoxy]-2-fluoropyridine | HCID 68430720 | 86% |
反応手順
2-(2-Bromoethyl)-1,3-dioxolane (2.49 ml, 19.9 mmol) and cesium carbonate (15.1 g, 46.4 mmol) were added to an N,N-dimethylacetamide solution (25 ml) of 6-fluoropyridin-3-ol (1.5 g, 13.3 mmol), and stirred under a nitrogen atmosphere at 100° C. for 12 hours. The reaction solution was cooled with ice, water and ethyl acetate were added, and the organic layer was washed with water and saturated saline water, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (Biotage, hexane:ethyl acetate=5:1 to 1:1) to obtain 5-[2-(1,3-dioxolan-2-yl)ethoxy]-2-fluoropyridine (2.43 g, yield: 86%) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08232284B2 |
|---|
| 出典データセット | uspto-grants-2012_07 |
|---|
| ORD ID | ord-06ef82f9cf31447cb63d9866125dd3cc |
|---|
| 出典メモ | uspto-grants-2012_07 |
|---|