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
Acetic acid (8 mL, 0.014 mmol) was added to an ambient temperature solution of 1-[4-(2,2-dimethyl-butyl)-1H-imidazol-2-yl]-2-[4-(1H-pyrazol-4-yl)phenyl]ethanamine (Example 37) (23 mg, 0.007 mmol), 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (26 mg, 0.014 mmol), 1-hydroxybenzotriazole (18 mg, 0.014 mmol) and sodium bicarbonate (57 mg, 0.07 mmol) in methylene chloride (5 mL) and N,N-dimethylformamide (0.5 mL). After stirring at ambient temperature overnight, the reaction mixture was diluted with water and extracted with ethyl acetate. The combined organic extracts were dried (magnesium sulfate) and concentrated in vacuo. Chromatography over silica eluting with 0-25% methanol/ethyl acetate afforded the title compound. (M+H) found: 422.
WORKUP
后处理
- extractionextracted with ethyl acetate
- dry with materialThe combined organic extracts were dried (magnesium sulfate)
- concentrationconcentrated in vacuo