関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | N-(p-acetylphenyl)acetamide | HCID 75937 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | N-[4-(2-Bromoacetyl)Phenyl]Acetamide | HCID 12364739 | 76.2% |
反応手順
To a suspension of 4′-acetamido-acetophenone 2 (21.84 g, 123 mmol) in acetic acid (184 mL), bromine (6.5 mL, 127 mmol) was added. The mixture was heated (inner temp: 52° C., oil bath temp: 60˜65° C.) with vigorous stirring until the suspension make a clear solution. The heating bath was rapidly removed, and the mixture was stirred at room temperature for 15 min and then stirred in an ice-water bath for 2 h(inner temp. 50° C.˜20° C.). The precipitation was filtrated, washed with 30% EtOH in water, and dried under reduced pressure to give 3 as a pale brown solid (24.0 g, 75% yield): MS(ES) m/e 257 [M+H].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07427623B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-f7f1377e5f9049a0a2fee1bedba4718b |
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| 出典メモ | uspto-grants-2008_09 |
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