HRID1803786
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 65 °C
PROCEDURE
实验过程
Ethyl 3-n-propylpyrazole-5-carboxylate (1.05 g, 5.8 mmol), 4′-bromomethyl-3′-fluorobiphenyl-2-carboxylic acid t-butyl ester (2.0 g, 5.8 mmol), and potassium carbonate (1.6 g, 11.5 mmol) were dissolved in DMF (10 mL). The mixture was stirred at 65° C. for 16 hours, then diluted with EtOAc. The organic layer was washed with saturated NaHCO3 and saturated aqueous NaCl, and dried over Na2SO4. The solvent was removed in vacuo and the residue was purified by flash chromatography (EtOAc in hexanes) to yield 1-(2′-t-butoxycarbonyl-3-fluorobiphenyl-4-ylmethyl)-5-propyl-1H-pyrazole-3-carboxylic acid ethyl ester (2.7 g).
WORKUP
后处理
- washThe organic layer was washed with saturated NaHCO3 and saturated aqueous NaCl
- dry with materialdried over Na2SO4
- customThe solvent was removed in vacuo
- customthe residue was purified by flash chromatography (EtOAc in hexanes)