HRID413419
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
N-[(4-Cyano-3-fluoro-phenyl)-(3-methyl-3H-imidazol-4-yl)-methylene]-2-methylpropanesulfinamide (1.50 g, 4.51 mmol) was dissolved in anhydrous THF (30 mL) at 0° C. and treated with a 3.0M solution of MeMgBr (4.50 mL, 13.5 mmol) in Et2O. After 15 min the reaction was quenched with aq. NH4Cl solution, diluted with saturated NaHCO3 solution and extracted with CH2Cl2 (3×). The combined organic layers were dried (MgSO4), filtered, concentrated, and recrystallized from 95% EtOAc/Hexane to give the title compound.
WORKUP
后处理
- customAfter 15 min the reaction was quenched with aq. NH4Cl solution
- additiondiluted with saturated NaHCO3 solution
- extractionextracted with CH2Cl2 (3×)
- dry with materialThe combined organic layers were dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customrecrystallized from 95% EtOAc/Hexane