関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 3,4-dihydro-5,7-dimethylnaphthalen-1(2H)-one | HCID 83619 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 1-Chloro-3,4-dihydronaphthalene-2-carboxaldehyde | HCID 76752 | — |
反応手順
3.5 mL of phosphorus oxychloride was added dropwise to 4.5 mL of dimethylformamide under ice cooling, after which the system was brought up to room temperature and stirred for 30 minutes. To this was added a solution of 5.0 g of 5,7-dimethyltetralone in 100 mL of chloroform, and the system was refluxed under heating overnight. After the reaction, water was added and the system was stirred for 30 minutes, after which the organic layer was washed first with a saturated sodium hydrogencarbonate aqueous solution and then with saturated brine, dried with magnesium sulfate, and then subjected to reduced-pressure solvent distillation, and the residue was refined by silica gel column chromatography (5% ethyl acetate/hexane) to obtain 5.8 g of 1-chloro-2-formyl-3,4-dihydronaphthalene in the form of a dark brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07384974B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-466dcdb5cf5342d7a5be6fa6df79e2fc |
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| 出典メモ | uspto-grants-2008_06 |
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