HRID2243138
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a stirred solution of the {2-ethyl-1-[1-(4-fluorobenzyl)-1H-1,2,4-triazol-5-yl]butyl}amine (0.133 g, 0.481 mmol) in CH2Cl2 (10 mL) was added Et3N (0.10 mL, 0.72 mmol) followed by 5-chlorothiophene-2-sulfonyl chloride (0.115 g, 0.529 mmol). The reaction mixture was stirred for 18 h, concentrated in vacuo, partitioned between 0.1N HCl and EtOAc. The organic extracts were dried (MgSO4), filtered and concentrated in vacuo. Column chromatography (SiO2, EtOAc/hexane, 3:7) provided pure material as a yellow solid in 60% yield.
WORKUP
后处理
- concentrationconcentrated in vacuo
- custompartitioned between 0.1N HCl and EtOAc
- dry with materialThe organic extracts were dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customColumn chromatography (SiO2, EtOAc/hexane, 3:7) provided pure material as a yellow solid in 60% yield