関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 反応物 | 5-(4-bromomethyl-3-chlorophenyl) 3-(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazole | HCID 21463648 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-(4-acetoxymethyl-3-chlorophenyl)-3-(2-chloro-6-fluorophenyl) 1-methyl-1H-1,2,4-triazole | HCID 21463681 | 51.1% |
反応手順
To N,N-dimethylformamide (200 ml) are added 5-(4-bromomethyl-3-chlorophenyl)-3(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazole (24.3 g) and potassium acetate (29.0 g), which are stirred at 130° C. for 3 hours. The reaction mixture is cooled to room temperature, poured into water and extracted with ethyl acetate. The organic layer is washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The concentrate is purified by silica gel column chromatography using mixed solvent of hexaneethyl acetate as eluent to give 11.8 g of desired compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05616594 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-8fa665d60d0042bb9c1b74ac3290d927 |
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| 出典メモ | uspto-grants-1997_04 |
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