関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Fluoroanisole | HCID 9975 | — |
| 反応物 | 2-Fluoro-4-(trifluoromethyl)benzoyl chloride | HCID 145580 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Nitrobenzene | HCID 7416 | — |
| 生成物 | (2-Fluoro-4-methoxy-phenyl)-(4-trifluoromethyl-phenyl)-methanone | HCID 22314037 | 24% |
反応手順
1.4 l of nitrobenzene were cooled in an ice bath and treated in succession at a maximum temperature of 6° C. with 492.6 g (3.656 mol) of aluminum chloride and 700 g (3.355 mol) of 4-trifluoromethyl-2-fluoro-benzoyl chloride in 350 ml of nitrobenzene. The mixture was stirred (15 min) and 427.5 g (3.388 mol) of 3-fluoroanisole were added slowly so that the temperature did not rise above 6° C. The solution was left to warm to room temperature, stirred 2 h at this temperature, poured on to ice-water (2.5 l) and extracted with methylene chloride. The organic phase was washed with water and concentrated. After crystallization from THF (1.2l)/hexane (4.2l), 237 g (24%) of (2-Fluoro-4-methoxy-phenyl)-(4-trifluoromethyl-phenyl)-methanone were obtained, MS: 298 (M).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07449483B2 |
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| 出典データセット | uspto-grants-2008_11 |
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| ORD ID | ord-4027d4f3cd5445eda91a4d13f65a5c5d |
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| 出典メモ | uspto-grants-2008_11 |
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