関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Sodium chlorodifluoroacetate | HCID 2734985 | — |
| 反応物 | 2-Bromo-5-hydroxypyridine | HCID 2762865 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-Bromo-5-(difluoromethoxy)pyridine | HCID 23120579 | 43% |
反応手順
Potassium carbonate (2.4 g, 17.3 mmols) and sodium chlorodifluoroacetate (4.2 g, 27.5 mmols) were added to a DMF (20 mL) solution of 2-bromo-5-hydroxypyridine (2.4 g, 13.8 mmols) and stirred overnight at 80° C. The reaction liquid was cooled to room temperature, added ether, washed with water and dried over anhydrous magnesium sulfate. Concentrating the solvent under reduced pressure, the resulting residue was purified on silica gel column chromatography (C-300; hexane:ethyl acetate=100:1-100:2) to provide the title compound (1.32 g, 43%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07732456B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-a7269e992a824e05b5d1f6a6b677604a |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|
