関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | N-(2-Acetylphenyl)acetamide | HCID 21306 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | N-[2-(2-bromoacetyl)phenyl]acetamide | HCID 2749459 | — |
反応手順
31 g (0.175 mol) of N-(2-Acetylphenyl)-acetamide (prepared by acylation of 2-aminoacetophenone with acetyl chloride as described by Fuerstner, Alois; Jumbam, Denis N.; Tetrahedron; 48; 29; 5991-6010, (1992)) was dissolved in 200 ml of glacial acetic acid. 127 ml of 33% strength HBr in glacial acetic acid was added and then, at room temperature, 8.75 ml (0.175 mol) of bromine was slowly run in. The mixture was stirred at room temperature overnight. The mixture was stirred into 1.5 l of ice-water, and the precipitated product was filtered off with suction, thoroughly washed with ice-water and dried in vacuo. The crude product contained, according to HPLC and NMR, some precursor and dibrominated product, but was pure enough (about 85% strength) for further reaction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06911453B2 |
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| 出典データセット | uspto-grants-2005_06 |
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| ORD ID | ord-686afb02858343efb828dce89b6416af |
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| 出典メモ | uspto-grants-2005_06 |
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