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Phenol → 2-chloro-6-phenyloxypyridine N-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phenol | HCID 996 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2,6-Dichloropyridine N-Oxide | HCID 817673 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 2-chloro-6-phenyloxypyridine N-oxide | HCID 54084605 | — |
反応手順
The 0.82 g (0.0050 moles) of 2,6-dichloropyridine N-oxide and 0.47 g (0.0050 moles of phenol was reacted with 0.200 g (0.0050 moles) of ground sodium hydroxide in 8.2 ml of DMSO at 80° C. for 6 hours to give 2-chloro-6-phenyloxypyridine N-oxide. It was reacted with 0.600 g (0.015 moles) of ground sodium hydroxide at 80° C. for 3.5 hours to give 1-hydroxy-6-phenyoxypyridine-2-(1H)-one. After cooling, it was added 74 ml of water and was adjusted with 6N HCl to pH 3. The water solution was extracted with dichloromethane (2×25 ml) and was dried over sodium sulfate. The dichloromethane solution was stripped in vacuo to give 1.29 g which was purified with Flash Chromatography (9:1 ethyl acetate:methanol):0.82 (65%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05424435 |
| 出典データセット | uspto-grants-1995_06 |
| ORD ID | ord-da3c1dfae2f54a75813ac8e0c23c8be8 |
| 出典メモ | uspto-grants-1995_06 |