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 | o-Fluorobenzaldehyde | HCID 67970 | — |
| 反応物 | 2-Methoxyethyl acetoacetate | HCID 89734 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 2-Methoxyethyl 2-acetyl-3-(2-fluorophenyl)-2-propenoate | HCID 59957778 | 70.4% |
反応手順
10 g (80 mmol) of 2-fluorobenzaldehyde are dissolved in 200 ml of isopropanol with 13 g (80 mmol) of 2-methoxyethyl acetoacetate. A freshly prepared solution of 1.0 ml of piperidine and 0.5 ml of glacial acetic acid in 10 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 300 ml of silica gel (eluent: toluene/ethyl acetate 100:1-10:1) to give 15 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-e157382722aa497aa3878591b7f42665 |
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| 出典メモ | uspto-grants-2003_10 |
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