HRID70077

反应详情

EQUATION

反应方程式

HRID 70077 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Phenylacetic acid (16 g, 117.6 mmol) and methanol (60 ml) were added to a 250 ml three-necked flask, followed by addition of 5 drops of concentrated sulphuric acid. The resulting solution was heated to reflux for 6 hours. Then, the mixture was cooled to room temperature, followed by adding n-butylamine (12 ml, 121.4 mmol), and heated to reflux for another 3 hours. After the reaction was completed, it was cooled to room temperature. Most of the solvent was removed by rotary vacuum evaporation, 30 ml of water was added thereinto, and the mixture was extracted with ethyl acetate (3×80 ml). The combined organic layer was dried over anhydrous magnesium sulfate, filtrated, and concentrated under reduced pressure to yield 15.9 g of N-n-butylphenylacetamide (white solid, yield: 70.4%).

WORKUP

后处理

  1. temperatureThe resulting solution was heated
  2. temperatureto reflux for 6 hours
  3. temperatureheated
  4. temperatureto reflux for another 3 hours
  5. temperatureit was cooled to room temperature
  6. customMost of the solvent was removed by rotary vacuum evaporation, 30 ml of water
  7. additionwas added
  8. extractionthe mixture was extracted with ethyl acetate (3×80 ml)
  9. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
  10. filtrationfiltrated
  11. concentrationconcentrated under reduced pressure