関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 2-chloro-N-(5-chloropyridin-2-yl)acetamide | HCID 5151148 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(5-chloropyridin-2-yl)-2-acetoxyacetamide | HCID 23062652 | 89.4% |
反応手順
2-Chloro-N-(5-chloropyridin-2-yl)acetamide (30.68 g) obtained in Reference Example 26(1) is dissolved in N,N-dimethylformamide (500 ml), thereto is added sodium acetate (24.55 g), and the mixture is stirred at 60° C. for 5 hours. The reaction solution is diluted with ethyl acetate, washed successively with water and saturated brine. The solution is dried over magnesium sulfate, treated with activated charcoal, and the filtrate is concentrated under reduced pressure. The resulting residue is suspended in n-hexane and crystals are collected by filtration, washed with n-hexane, and dried to give N-(5-chloropyridin-2-yl)-2-acetoxyacetamide (30.58 g). APCI-MS M/Z:229/231[M+H]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07605158B2 |
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| 出典データセット | uspto-grants-2009_10 |
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| ORD ID | ord-69929170c9814fa581953b4d1a5fee46 |
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| 出典メモ | uspto-grants-2009_10 |
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