反应详情

温度

50 °C

To a solution of 1-methyl-1H-pyrazole-5-carboxylic acid (300 mg, 2.4 mmol) in DMF (7 mL) was added CDI (372 mg, 2.6 mmol), and the reaction mixture was heated to 50° C. for two hours. Then the mixture was cooled to −5° C., a solution of ethyl 2-(thiophen-3-yl)acetate (444 mg, 2.6 mmol) in DMF (1 mL) was added to the mixture and NaH (330 mg, 8.2 mmol) was added in portions. The mixture was stirred at 0° C. for 10 minutes, then warmed to room temperature and stirred for 1 hour. Ice water was added, followed by a standard aqueous/EtOAc workup. Crude was purified by column chromatography (PE:EtOAc=5:1) (150 mg, yield: 22.7%).

1. temperatureThen the mixture was cooled to −5° C.
2. additionwas added in portions
3. temperaturewarmed to room temperature
4. stirringstirred for 1 hour
5. customCrude was purified by column chromatography (PE:EtOAc=5:1) (150 mg, yield: 22.7%)