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Water → 2-Bromo-5-(4-t-butylphenyl)-4-hydroxy-3-methylcarbonylthiophene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 2-(4-t-Butylphenyl)-3-hydroxy-4-methylcarbonylthiophene | HCID 44207289 | — |
| 触媒 | Benzoyl Peroxide | HCID 7187 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-Bromo-5-(4-t-butylphenyl)-4-hydroxy-3-methylcarbonylthiophene | HCID 67050460 | 86% |
反応手順
2-(4-t-butylphenyl)-3-hydroxy-4-methylcarbonylthiophene (2.66 g, 9.7 mmol), N-bromosuccinimide (1.73 g, 9.7 mmol) and benzoyl peroxide (153 mg, 0.63 mmol) were heated with reflux for 2 hours in 65 ml of chloroform. Water was added, and the reaction solution was extracted three times with chloroform, and the organic layer was washed with a saturated aqueous sodium chloride solution, and then dried over anhydrous sodium sulfate. The obtained organic layer was concentrated, and then purified with a silica gel column chromatography (n-hexane/chloroform=3/2) to obtain the desired product as a yellow solid (2.93 g, yield 86%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07576115B2 |
| 出典データセット | uspto-grants-2009_08 |
| ORD ID | ord-dd552c7d2f754aa7ab09c0a762b06ad5 |
| 出典メモ | uspto-grants-2009_08 |