関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,3-Cyclohexanedione | HCID 10434 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | Sulcotrione | HCID 91760 | — |
| 反応物 | 2-Chloro-4-(methylsulfonyl)benzoic acid | HCID 735863 | — |
| 触媒 | 1H-1,2,4-Triazole | HCID 9257 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Benzoyl chloride, 2-chloro-4-(methylsulfonyl)- | HCID 11128804 | 83.6% |
反応手順
2-(2-Chloro-4-methanesulphonylbenzoyl)-1,3-cyclohexanedione from the acid chloride. 2-Chloro-4-methanesulphonylbenzoyl chloride (5 g) was prepared by the reaction of 2-chloro-4-methanesulphonylbenzoic acid with thionyl chloride. The acid chloride was dissolved in acetonitrile (40 ml). A mixture of 1,3-cyclohexanedione (2.24 g), potassium carbonate (6.9 g) and acetonitrile (40 ml) was stirred at room temperature for 4 hours. To this solution was added the acid chloride solution over 10 min and allowed to stir 1 hour. 1,2,4-Triazole (0.07 g) was then added and the mixture allowed to stir 16 hours at room temperature. The solvent was removed and the residue was dissolved in water and acidified. The product was extracted into dichloromethane and the solvent was dried then evaporated to give the desired product in 83.6% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06218579B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-4c98c7e96af84206acf08bce6722fb9e |
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| 出典メモ | uspto-grants-2001_04 |
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