関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 反応物 | 4-bromo-5-(4-chlorobutyl)-1-ethyl-1H-pyrazole-3-carbonitrile | HCID 66958265 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(4-bromo-5-cyano-2-ethyl-2H-pyrazol-3-yl)butyl acetate | HCID 66958636 | 80.5% |
反応手順
Potassium acetate (1.69 g, 17.2 mmol), sodium iodide (255 mg, 1.7 mmol), and DMF (17 mL) were added to 4-bromo-5-(4-chlorobutyl)-1-ethyl-1H-pyrazole-3-carbonitrile (1.0 g, 3.4 mmol, prepared as described in Parts A-E of Example 19), and the reaction was heated at 100° C. for two hours under a nitrogen atmosphere and allowed to cool to ambient temperature. Water was added, and the resulting mixture was extracted with diethyl ether. The combined extracts were washed with brine, dried over magnesium sulfate, filtered, and concentrated under reduced pressure. The crude product was purified by chromatography on a HORIZON HPFC system (40+M cartridge, eluting with hexanes/ethyl acetate in a gradient from 90:10 to 60:40) to provide 0.86 g of 4-(4-bromo-5-cyano-2-ethyl-2H-pyrazol-3-yl)butyl acetate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09145410B2 |
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| 出典データセット | uspto-grants-2015_09 |
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| ORD ID | ord-ccbbcce73c014a1791d3fa6e720f7fcb |
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| 出典メモ | uspto-grants-2015_09 |
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