化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Carbonate → 1-(4-Pyridinyl)-5-methyl-2-pyridone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Hydroxy-5-methylpyridine | HCID 70482 | — |
| 反応物 | 4-Bromopyridinium chloride | HCID 88100 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Ammonia | HCID 222 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(4-Pyridinyl)-5-methyl-2-pyridone | HCID 9794088 | — |
反応手順
Compound 22 was synthesized by condensation of 5-methyl-2(1H)-pyridone (327.4 mg, 3 mmol) with 4-bromopyridine hydrochloride (778 mg, 4 mmol) in the presence of CuI (60 mg, 0.3 mmol) and K2CO3 (1.36 g, 10 mmol) in DMF (3 ml) at 135° C. overnight. The reaction mixture was diluted with 10% ammonia (15 ml) and extracted with ethyl acetate. Organic extract was washed with saturated sodium chloride, dried over magnesium sulfate and evaporated. Column chromatography (5% MeOH-DCM) afforded 197 mg (35%) of the target compound as a yellowish solid. The 1H NMR spectra was consistent with the structure of Compound 22.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08741936B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-20a96b4fa2614b0ba30644ffbd2d5958 |
| 出典メモ | uspto-grants-2014_06 |