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Thiophenol → 2-chloro-6-thiophenylpyridine N-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thiophenol | HCID 7969 | — |
| 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-thiophenylpyridine N-oxide | HCID 86748730 | — |
反応手順
The 1.64 g (0.010 moles) of 2,6-dichloropyridine N-oxide and 1.11 g (99%) (0.010 moles) of thiophenol was reacted with 0.400 g (0.010 moles) of ground sodium hydroxide of 16.4 ml of DMSO at 80° C. for 5 hours to give 2-chloro-6-thiophenylpyridine N-oxide. It was reacted with 1.20 g (0.030 moles) of ground sodium hydroxide at 80° C. for 2.5 hours to give 1-hydroxy-6-thiophenylpyridine-2-(1H)-one. After cooling, it was added 148 ml of water and was adjusted with 6N HCl to pH 3. The precipitate was filtered, washed with water and washed with hexanes to give 1.64 g (75%). It was recrystallized from ethanol: mp 180°-181° C.
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-dd733e1a9b8e43559d9f6fc67ca8840f |
| 出典メモ | uspto-grants-1995_06 |