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Hydrochloric Acid → Methyl 5-(4-chlorophenyl)-5-oxovalerate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Chlorobenzene | HCID 7964 | — |
| 反応物 | Methyl 4-chloroformylbutyrate | HCID 73916 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | Methyl 5-(4-chlorophenyl)-5-oxovalerate | HCID 10966649 | 82.2% |
反応手順
Chlorobenzene (8.13 ml, 79.9 mmol) was dissolved in 100 ml of 1,2-dichloroethane, and 21.3 g (160 mmol) of aluminum trichloride and 12.15 ml (87.9 mmol) of methyl 4-(chloroformyl)butyrate were added thereto, followed by stirring the mixture at room temperature overnight. The reaction solution was poured into hydrochloric acid, and extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was then distilled off under reduced pressure. The resulting residue was purified by silica-gel column chromatography (eluent: a mixture of 4% ethyl acetate and hexane) to obtain 15.8 g of the above-mentioned compound (yield 82%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05646283 |
| 出典データセット | uspto-grants-1997_07 |
| ORD ID | ord-3f0f68dd45e943b8a27883536a64ad75 |
| 出典メモ | uspto-grants-1997_07 |