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2-Hydrazinopyridine → 3,5-dimethyl-1-pyridin-2-yl-1H-pyrazole-4-carboxylic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Hydrazinopyridine | HCID 78645 | — |
| 反応物 | Ethyl 2-acetylacetoacetate | HCID 79063 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 3,5-dimethyl-1-pyridin-2-yl-1H-pyrazole-4-carboxylic acid ethyl ester | HCID 9856256 | 97.2% |
反応手順
Dissolve 2-acetyl-3-oxobutyric acid ethyl ester (20.74 g, 0.120 mol) and 2-pyridylhydrazine (14.5 mL, 0.133 mol) in acetic acid (160 mL) and stir the mixture for 18 hr. Concentrate, dilute with DCM, wash with saturated sodium bicarbonate, dry (sodium sulfate), filter and concentrate to give 3,5-dimethyl-1-pyridin-2-yl-1H-pyrazole-4-carboxylic acid ethyl ester as an oil (28.6 g, 97%). MS (m/z): 246 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07910588B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-6e784c4a9e6a48a6b1c0e590182260a1 |
| 出典メモ | uspto-grants-2011_03 |