反应详情

To a slurry of 3.0g (0.075 mol) of sodium hydride in 30 mL of DMF at room temperature was added 10g (0.069 mol) of 4-phenyl-1H-pyrazole of example 1. The mixture was stirred 1 hr and 7.8 mL (0.07 mol) of ethyl bromoacetate was added with cooling. The reaction was stirred 3 hr at room temperature, briefly at 100° C. and was poured onto ice. The product was filtered off, rinsed with water, dried, and washed with hexane to yield 14.0g of ethyl 4-phenyl-1H-pyrazole-1-acetate.

1. temperaturewith cooling
2. stirringThe reaction was stirred 3 hr at room temperature, briefly at 100° C.
3. additionwas poured onto ice
4. filtrationThe product was filtered off
5. washrinsed with water
6. customdried
7. washwashed with hexane