HRID840584

反应详情

EQUATION

反应方程式

HRID 840584 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. additionwas added
  2. washthe organic phase washed with 1N aqueous hydrochloric acid (twice), water (twice) and saturated aqueous sodium bicarbonate (thrice)
  3. dry with materialThe resulting organic solution was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated