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Sodium Bicarbonate → 5-ethoxy-2-(2-fluorophenyl)-2,4-dihydro-3H-pyrazol-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Hydrazine, (2-fluorophenyl)-, hydrochloride (1:1) | HCID 2723910 | — |
| 反応物 | Ethyl beta-amino-beta-ethoxyacrylate hydrochloride | HCID 53395434 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5-ethoxy-2-(2-fluorophenyl)-2,4-dihydro-3H-pyrazol-3-one | HCID 67468970 | — |
反応手順
(2-Fluorophenyl)hydrazine hydrochloride (1.00 g, 6.15 mmol) was suspended in ethanol (10 mL), treated with ethyl 3-amino-3-ethoxyacrylate hydrochloride (1.20 g, 6.15 mmol, 1.00 equiv), and placed into a preheated oil bath at 70° C. for 5 hours. The mixture was cooled to ambient temperature, poured into saturated aqueous sodium bicarbonate (100 mL), and extracted with ethyl acetate (3×75 mL). The combined organic extracts were dried with sodium sulfate, filtered, and concentrated in vacuo. The residue was purified by silica gel chromatography (100:0 to 0:100 hexanes:ethyl acetate), providing the titled compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08507494B2 |
| 出典データセット | uspto-grants-2013_08 |
| ORD ID | ord-39dd79331e9a4fb28dcd15ed78f95851 |
| 出典メモ | uspto-grants-2013_08 |