反应详情

温度

100 °C

To a solution of ethyl 3-iodo-1H-pyrazole-4-carboxylate (1.10 g, 3.91 mmol) in tert-butanol (5 mL) was added sulfuric acid (0.40 mL, 4.18 mmol, 18 M). The reaction was heated to 100° C. and stirred for 3 hours. The reaction was cooled to room temperature and diluted with ethyl acetate (100 mL) and water (25 mL). The pH was adjusted to 8 with saturated aqueous sodium bicarbonate. The layers were separated and the organics were dried over sodium sulfate, filtered, and concentrated. Purification by flash column chromatography (7-60% ethyl acetate/heptanes) gave 2 regioisomeric products.

1. temperatureThe reaction was cooled to room temperature
2. customThe layers were separated
3. dry with materialthe organics were dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customPurification by flash column chromatography (7-60% ethyl acetate/heptanes)
7. customgave 2 regioisomeric products