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Cesium carbonate → 3-(2-Fluoro-4-nitrophenoxy)-2,6-dimethyl-pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2,6-Dimethyl-3-pyridinol | HCID 70732 | — |
| 反応物 | 1,2-Difluoro-4-nitrobenzene | HCID 123053 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-(2-Fluoro-4-nitrophenoxy)-2,6-dimethyl-pyridine | HCID 59287319 | — |
反応手順
To a solution of 2,6-dimethyl-3-pyridinol (3 g, 24.35 mmol) in THF (30 ml) at r.t., were added Cs2CO3 (15.87 g, 48.71 mmol) and 3,4-difluoro-1-nitro-benzene (3.87 g, 24.35 mmol). The reaction mixture was heated at reflux for 2 h. After cooling to r.t. the solids were filtered off and the filtrate was evaporated to dryness. The crude product was purified by column chromatography (silica gel; DCM/7M solution of NH3 in MeOH up to 2% as eluent). The desired fractions were collected and concentrated in vacuo to yield intermediate compound D21 (5.88 g, 92%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08716480B2 |
| 出典データセット | uspto-grants-2014_05 |
| ORD ID | ord-9b3d60d6ddc74e5a8519efaf65c9e638 |
| 出典メモ | uspto-grants-2014_05 |