関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2,6-Dichloro-4'-methoxy-2'-methyl-benzophenone | HCID 54505258 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5'-Bromo-2,6-dichloro-4'-methoxy-2'-methyl-benzophenone | HCID 54309764 | — |
反応手順
A solution of bromine (0.25 ml in 3 ml of trichloromethane) is added dropwise to a stirred solution of 2,6-Dichloro-4'-methoxy-2'-methyl-benzophenone (1.5 g; 5 mmol in 5 ml of trichloromethane), followed by 15 minutes of stirring at 20° C. The mixture is shaken with water, sodium hydrogencarbonate solution and water. The organic phase is dried and evaporated. The residue is purified by chromatography (flash column filled with 30 g of silicagel, elution with petrolether/ethylacetate changing from 20:1 to 9:1, 8:2, 7:3 (v/v) . After evaporation, the residue crystallises when treated with petrolether/toluene to give white crystalls (0.45 g; 24% y); mp. 159° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05922919 |
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| 出典データセット | uspto-grants-1999_07 |
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| ORD ID | ord-0b9ab888606047f4b7180c395a3a81cf |
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| 出典メモ | uspto-grants-1999_07 |
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