関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Bromo-2-fluoroaniline | HCID 123050 | — |
| 反応物 | 2-Chloro-6-(trifluoromethoxy)-1,3-benzothiazole | HCID 10037924 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | N-(4-bromo-2-fluorophenyl)-N-(6-trifluoromethoxy-1,3-benzothiazol-2-yl)amine | HCID 21985778 | 58.1% |
反応手順
In a 250-mL round-bottom flask, 2-chloro-6-trifluoromethoxy-1,3-benzothiazole (5.36 g, 21.14 mmol) and 4-bromo-2-fluoroaniline (4.82 g, 25.36 mmol) were combined in 100 mL n-butanol containing 1% 4.0 M HCl in dioxane, and heated at 90° C. overnight. The mixture was cooled to rt and the solvent was removed under reduced pressure. Ethyl acetate (50 mL) was added, and the mixture was ultrasonicated by suspending the flask in an ultrasonication bath for 30 minutes. The mixture was filtered, and the filtrate was concentrated under reduced pressure. Acetonitrile (50 mL) was added to the mixture, which was then ultrasonicated for 30 minutes and then filtered to provide the product as a white solid (5 g, 58%). LC-MS m/z 409.1 (MH+), ret. time 4.02 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07423156B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-90ba5aab8e7741e6b17339b8382e4634 |
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| 出典メモ | uspto-grants-2008_09 |
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