関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2,3-Dichloroanisole | HCID 16126 | — |
| 反応物 | 4-Chloro-2-fluorobenzoyl chloride | HCID 2773601 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 2,3-Dichloro-4-methoxy-4'-chloro-2'-fluorobenzophenone | HCID 14097267 | — |
反応手順
To a mixture of 46 g of 4-chloro-2-fluorobenzoyl chloride and 38.9 g of 2,3-dichloroanisole in 150 ml of 1,2-dichloroethane, 32 g of AlCl3 is added gradually. The mixture is warmed to 40° C. with a vigorous evolution of gas. The mixture is poured into concentrated HCl and ice. The organic layer is separated and the aqueous layer is extracted with additional organic solvent. The combined organic extracts are washed with water, dried over Na2SO4 and evaporated. The crude product is triturated with hexane to give 2,3-dichloro-4-methoxy-4'-chloro-2'-fluorobenzophenone. An analytical sample is recrystallized from EtOH, mp 115°-116° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04728662 |
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| 出典データセット | uspto-grants-1988_03 |
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| ORD ID | ord-bc590864a6fc47a98ea3d7f652422ddd |
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| 出典メモ | uspto-grants-1988_03 |
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