関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Chloro-5-(chloromethyl)pyridine | HCID 155479 | — |
| 反応物 | 2-Chloro-4-(3-bromophenoxy)phenol | HCID 19798096 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Chloro-5-[4-(3-bromophenoxy)-2-chlorophenoxy]methylpyridine | HCID 19798098 | — |
反応手順
To a solution of 0.07 g of sodium hydride (60% oil dispersion) in 10 ml of N,N-dimethylformamide, there is added dropwise a solution of 0.50 g of 2-chloro-4-(3-bromophenoxy)phenol in 3 ml of N,N-dimethylformamide with stirring and ice-cooling. After 30 minutes, a solution of 0.27 g of 2-chloro-5-chloromethylpyridine in 5 ml of N,N-dimethylformamide is added thereto at room tempearture, followed by stirrring at the same temperature for 10 hours. The reaction mixture is poured into ice-water and extracted twice with 100 ml of ethyl acetate. The extracts are combined together, washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue is subjected to silica gel chromatography to give 2-chloro-5-[4-(3-bromophenoxy)-2-chlorophenoxy]methylpyridine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05243087 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-1b4f35597bfc40f99c6612fc401f6e22 |
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| 出典メモ | uspto-grants-1993_09 |
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