関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3'-Cyano-4'-isobutylacetophenone | HCID 22228006 | — |
| 反応物 | Sodium Hypochlorite | HCID 23665760 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Cyano-4-isobutylbenzoic acid | HCID 22228175 | — |
反応手順
Subsequently, 10% aqueous sodium hypochlorite solution (370 ml) containing sodium hydroxide (8 g) and methanol (5 ml) was heated to 60° C. 3′-Cyano-4′-isobutylacetophenone (20 g) was added thereto by portions and the mixture was stirred for 1 h. The reaction mixture was cooled to room temperature and dilute hydrochloric acid was added, which was followed by extraction with chloroform. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. n-Hexane was added to the residue to allow crystallization. The crystals were recrystallized from a mixed solvent of ethyl acetate-n-hexane to give 3-cyano-4-isobutylbenzoic acid (8.5 g), melting point: 118° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07015218B1 |
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| 出典データセット | uspto-grants-2006_03 |
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| ORD ID | ord-4c07db60f7244724ad7624ce2f02fc44 |
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| 出典メモ | uspto-grants-2006_03 |
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