関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-(2-Phenylpyrimidin-5-yl)ethanone | HCID 22631072 | — |
| 反応物 | Tetra-n-butylammonium tribromide | HCID 23500184 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Bromo-1-(2-phenylpyrimidin-5-yl)ethanone | HCID 59252454 | 79.4% |
反応手順
To a solution consisting of 1-(2-phenylpyrimidin-5-yl)ethanone (Step A, 700 mg, 3.5 mmol) in dichloromethane (25 mL) was added tetrabutylammonium tribromide (1.87 g, 3.90 mmol). The reaction mixture was sealed with a screw top and warmed at 40° C. for 5 hours and allowed to cool to room temperature over a weekend. The pale yellow precipitate formed was collected on a filter and washed with 1:1 dichloromethane-hexane to afford the title intermediate (770 mg, 79%); Rf 0.31 with 9:1 v/v hexanes-ethyl acetate; MS (ESI+) m/z 279, 277 (M+1, Br isotopes).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536185B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-49ef573663a4412a8513614681ec736e |
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| 出典メモ | uspto-grants-2013_09 |
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