関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 2,4-Difluorobenzaldehyde | HCID 73770 | — |
| 反応物 | 2-Methoxyethyl acetoacetate | HCID 89734 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 2-Methoxyethyl 2-acetyl-3-(2,4-difluorophenyl)-2-propenoate | HCID 54334891 | 50.3% |
反応手順
5.0 g (35 mmol) of 2,4-difluorobenzaldehyde are dissolved in 100 ml of isopropanol with 5.7 g (35 mmol) of 2-methoxyethyl acetoacetate. A freshly prepared solution of 1.0 ml of piperidine and 0.5 ml of glacial acetic acid in 5 ml of isopropanol is added to this solution and it is stirred overnight at 40° C. The mixture is concentrated, the residue is taken up in toluene, the solution is concentrated again and the residue is purified by filtration on 100 ml of silica gel (eluent: toluene/ethyl acetate 100:1) to give 5 g of the target compound as a yellow oil which is immediately reacted further.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06630494B2 |
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| 出典データセット | uspto-grants-2003_10 |
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| ORD ID | ord-5c514f623e7d418ba1dfdce3b83ddd22 |
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| 出典メモ | uspto-grants-2003_10 |
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