関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Chloro-2-methylphenol | HCID 14855 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | Benzoyl chloride, 2-chloro-4-(methylsulfonyl)- | HCID 11128804 | — |
| 溶媒 | 1,1,2,2-Tetrachloroethane | HCID 6591 | — |
| 生成物 | 2,5'-Dichloro-2'-hydroxy-3'-methyl-4-methylsulfonylbenzophenone | HCID 18544637 | 60% |
反応手順
5.06 g of 2-chloro-4-methylsulfonylbenzoyl chloride are added in portions at room temperature to a mixture of 2.85 g of 4-chloro-2-methylphenol and 5.40 g of aluminum chloride in 100 ml of 1,1,2,2-tetrachloroethane, and the mixture is subsequently refluxed for 7 hours. When cold, the reaction mixture is poured onto 200 g of ice and 500 ml of concentrated hydrochloric acid. The organic phase is separated off, and the aqueous phase is extracted twice using 50 ml of dichloromethane. The combined organic phases are washed until neutral, dried over magnesium sulfate and evaporated. Recrystallization from a mixture of ethyl acetate and diisopropyl ether gives 4.2 g (60% of theory) of 2,5'-dichloro-2'-hydroxy-3'-methyl-4-methylsulfonylbenzophenone in the form of colorless crystals with a melting point of 175°-180° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05843869 |
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| 出典データセット | uspto-grants-1998_12 |
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| ORD ID | ord-02f59a759fdf44f58589e412cf2950bc |
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| 出典メモ | uspto-grants-1998_12 |
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