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ethyl 4-bromo-1-tosyl-1H-pyrazole-3-carboxylate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
94%
With N-Bromosuccinimide; In ethyl acetate; at 25℃; for 12h;
In the drying tube was added 70mg of 3-pyrazolylEthyl acetateAnd 178mg of methyl benzene sulfinateSodium, added 267mg of NBS. 2mL ethyl acetate was then added to dissolve the solid, the reaction solution was stirred at 25 12 hours. After completion of the reaction, ethyl acetate and water extraction, the resulting organic phase was concentrated on a rotary evaporator, silica gel column (ethyl acetate and petroleum ether, the volume ratio of 1: 3) to give 175 mg of product, 94percent yield , the following reaction formula:
72%
With N-Bromosuccinimide; In ethyl acetate; at 25℃; for 12h;
General procedure: Pyrazoles 4 (0.5 mmol), sodium sulfinate 2 (1.0 mmol) and NBS or NIS (1.5 mmol) were dissolved in 2 mL of EtOAc solvent. the reaction mixture was stirred at room temperature under air for 12 h. After the reaction, the resulting mixture was extracted with EtOAc. The combined organic phase was dried over anhydrous Na2SO4 and the solvent was then removed under vacuum. The residue was purified by flash column chromatography on silica gel (petroleum ether/ethyl acetate, 3:1) to afford the corresponding product.
Chemistry
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Material Science
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