反应详情

温度

90 °C

A mixture of 1-butyl-5-methyl-1H-pyrazole-3-carboxamide (6.9 g, 38 mmol) and phosphorous oxychloride (34.0 mL) was heated at 90° C. under a nitrogen atmosphere for two hours and then allowed to cool to ambient temperature overnight. The reaction was poured into ice water (300 mL); concentrated ammonium hydroxide (115 mL) was added. The mixture was extracted with chloroform (3×), and the combined extracts were dried over magnesium sulfate, filtered, and concentrated under reduced pressure to provide 6.58 g of 1-butyl-5-methyl-1H-pyrazole-3-carbonitrile as a pale yellow oil.

1. temperatureto cool to ambient temperature overnight
2. extractionThe mixture was extracted with chloroform (3×)
3. dry with materialthe combined extracts were dried over magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure