HRID1242385

反应详情

EQUATION

反应方程式

HRID 1242385 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

1.0 g (4.0 mmol) of 3-(1-ethoxycarbonyl-1-methyl-ethoxy)-benzoic acid was dissolved in 50 ml of methylene chloride; then, 1.5 ml (4.0 mmol) of a methylamine-solution in ethanol was added. The reaction mixture was cooled down to 0° C. and 0.91 g (4.8 mmol) of N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride and 1.50 g (11.9 mmol) of 4-dimethylaminopyridine were added. After stirring for two hours at ambient temperature, it was poured into crashed ice/HCl (1N) and extracted twice with MeCl2. The combined organic phases were washed with water and brine and dried over anhydrous magnesium sulfate. After evaporation of the solvent, the crude product was purified by flash chromatography (SiO2, MeCl2/MeOH) to give 0.97 g of the title compound in form of colorless needles.

WORKUP

后处理

  1. additionit was poured
  2. extractionextracted twice with MeCl2
  3. washThe combined organic phases were washed with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customAfter evaporation of the solvent
  6. customthe crude product was purified by flash chromatography (SiO2, MeCl2/MeOH)