関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3,3-Diethoxy-1-propene | HCID 62477 | — |
| 反応物 | 4-Iodobenzaldehyde | HCID 96657 | — |
| 触媒 | Tetrabutylammonium Chloride | HCID 70681 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | ETHYL 3-(4-FORMYLPHENYL)PROPANOATE | HCID 12169276 | 711.8% |
反応手順
To a solution of 4-iodobenzaldehyde (0.116 g, 0.5 mmol), acrolein diethylacetal (0.3 mL, 1.5 mmol), tetra-n-butylammonium chloride (0.139 g, 0.5 mmol) and triethylamine in anhydrous dimethylformamide (2 mL), palladium acetate (0.003 g, 0.015 mmol) was added. The reaction mixture was heated at 90° C. and stirred for 16 h. The reaction mixture was diluted with 2 N hydrochloric acid and extracted with diethyl ether. The solvent was evaporated in vacuo to leave a residue which was purified by column chromatography (silica gel) employing 1-5% ethyl acetate in hexane as eluents to obtain 3-(4-formyl-phenyl)-propionic acid ethyl ester (0.734 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08889698B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-31b131695bb84240b49d7a88697497be |
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| 出典メモ | uspto-grants-2014_11 |
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