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m-Chloroperbenzoic acid → 3-bromo-5-(1-hydroxy-1-methylethyl)pyridine-N-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | Calcium Hydroxide | HCID 6093208 | — |
| 反応物 | 2-(5-Bromo-3-pyridyl)propan-2-ol | HCID 22391966 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 3-bromo-5-(1-hydroxy-1-methylethyl)pyridine-N-oxide | HCID 22714295 | — |
反応手順
To a solution of 3-bromo-5-(1-hydroxy-1-methylethyl)pyridine from Step 1 (3.1 mmol) in chloroform (10 mL) was added m-chloroperoxybenzoic acid 70% (1.5 eq) and the resulting mixture was stirred at room temperature for 18 hours. An excess of calcium hydroxide was added and after stirring for 5 minutes, the mixture was filtered through celite and the filtrate was evaporated. The crude material was chromatographed on silica gel eluting with 10% ethanol in methylene chloride (saturated with ammonia) to afford the 3-bromo-5-(1-hydroxy-1-methylethyl)pyridine-N-oxide compound as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06743802B2 |
| 出典データセット | uspto-grants-2004_06 |
| ORD ID | ord-5084663d34d84e07a461dca7efbaf530 |
| 出典メモ | uspto-grants-2004_06 |