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Water → 3-methyl-5-nitro-2-(1H-pyrazol-1-yl)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Pyrazole | HCID 1048 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | 6-Chloro-5-methylpyridin-3-amine | HCID 12295607 | — |
| 生成物 | 3-methyl-5-nitro-2-(1H-pyrazol-1-yl)pyridine | HCID 63811636 | — |
反応手順
Cesium carbonate (75 mg) and pyrazole (12 mg) were added to an N,N-dimethylacetamide (5 ml) solution containing 6-chloro-5-methylpyridin-3-amine (12 mg), followed by reflux for 3.5 hours. Water was added to the reaction solution, followed by extraction with ethyl acetate. The resultant was washed with saturated saline and dried over anhydrous sodium sulfate. Subsequently, the solvent was distilled away under reduced pressure, the obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=1:0 to 10:1), and a light yellow solid of 3-methyl-5-nitro-2-(1H-pyrazol-1-yl)pyridine (12 mg) was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08895585B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-735b1e9d3daa46ca9a9131f41cfffbec |
| 出典メモ | uspto-grants-2014_11 |