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Water → 2-(3,5-dimethyl-1H-pyrazol-1-yl)pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3,5-Dimethylpyrazole | HCID 6210 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Chloropyrimidine | HCID 74404 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(3,5-dimethyl-1H-pyrazol-1-yl)pyrimidine | HCID 30464906 | 69% |
反応手順
NaH (0.594 g, 14.84 mmol) was suspended in THF (10 mL), and 3,5-dimethylpyrazole (1.091 g, 11.35 mmol) was slowly added and stirred for one hour at room temperature. 2-Chloropyrimidine (1 g, 8.73 mmol) was slowly added to the mixture and refluxed for three hours. Completion of the reaction was confirmed by TLC, and then water (5 mL) was added to the mixture. The solvent was distilled off and the residue was extracted with ethyl acetate twice. The organic phase was washed with saturated brine and dried over magnesium sulfate. The solvent was then distilled off and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:2→ethyl acetate) to give 1.05 g of the title compound (yield 69%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08563552B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-80403708ca76439d9aab5d6698a31937 |
| 出典メモ | uspto-grants-2013_10 |