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
PROCEDURE
实验过程
40 mg of 5% palladium on carbon were added to a solution of 500 mg (2.0 mmol) of 3-[5-(4-fluoro-phenyl)-thiophen-2-yl]-acrylic acid in 20 ml of tetrahydrofuran, and the reaction mixture was hydrogenated at atmospheric pressure and room temperature for 24 h. 10 ml of methanol and 40 mg of 5% palladium on carbon were added and the reaction mixture was hydrogenated at atmospheric pressure and room temperature for further 24 hours. 10 ml of acetic acid were added and the reaction mixture was hydrogenated at atmospheric pressure and room temperature for another 24 h. The mixture was filtered and evaporated, and the product was purified by preparative RP HPLC eluting with a gradient of 0 to 100% acetonitrile in water (+0.01% TFA). After lyophilization, the product was obtained as a solid. Yield: 400 mg.
WORKUP
后处理
- waitthe reaction mixture was hydrogenated at atmospheric pressure and room temperature for further 24 hours
- waitthe reaction mixture was hydrogenated at atmospheric pressure and room temperature for another 24 h
- filtrationThe mixture was filtered
- customevaporated
- customthe product was purified by preparative RP HPLC
- washeluting with a gradient of 0 to 100% acetonitrile in water (+0.01% TFA)
- customAfter lyophilization, the product was obtained as a solid