HRID840584
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
A solution containing 500 mg (2.65 mmol) of 3-nitrobenzylamine in 20 mL of dichloromethane was stirred at room temperature as 463 mg (3.18 mmol) of 5-methyl-3-isoxazoyl chloride was added. To this solution was added 0.92 mL (6.62 mmol) of triethylamine. The reaction was stirred an additional 1 hour at room temperature, diluted with 75 mL of ethyl acetate and the organic phase washed with 1N aqueous hydrochloric acid (twice), water (twice) and saturated aqueous sodium bicarbonate (thrice). The resulting organic solution was dried over sodium sulfate, filtered, and concentrated to give 550 mg (79%) of the title compound as a yellow solid. MS(FD) m/z 261 (M+).
WORKUP
后处理
- additionwas added
- washthe organic phase washed with 1N aqueous hydrochloric acid (twice), water (twice) and saturated aqueous sodium bicarbonate (thrice)
- dry with materialThe resulting organic solution was dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated