関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | 2-Bromo-6-methylpyridine | HCID 79205 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Bromo-6-methylpyridine 1-oxide | HCID 3652084 | 75.2% |
反応手順
Hydrogen peroxide (30%, 1.76 mL, 17.4 mmol) was added to a solution of 2-bromo-6-methyl-pyridine (1.0 g, 5.80 mmol) in acetic acid (20 mL), and heated for 24 h at 90° C. The reaction mixture was cooled to ambient temperature, and partitioned between dichloromethane and water. The aqueous phase was separated and extracted with dichloromethane. The combined organic phases were washed thoroughly with water and dried over anhydrous sodium sulfate. Concentration in vacuo afforded 2-bromo-6-methyl-pyridine 1-oxide (820 mg, 75%) as a brown liquid which was used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08524705B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-e7ec2c1329ad4d029fdc28cbdb7d8051 |
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| 出典メモ | uspto-grants-2013_09 |
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