HRID1975539

反应详情

EQUATION

反应方程式

HRID 1975539 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A 100 ml autoclave was charged with 1.96 g (9.8 mmol) of 1-(3,5-dimethylphenoxy)-2-chloropropane, 10 ml of ethanol and 0.2 g of sodium iodide, and then 40 ml of a 28% ammonia aqueous solution was added. The mixture was continuously stirred at 130° C. for 8 hours to complete the reaction. After allowed to cool, the reaction mixture was transferred into a 500 ml beaker with 50 ml of water and 20 ml of diethyl ether. A 20% hydrochloric acid aqueous solution was added to the reaction mixture until it became acidic, and the mixture was washed with 20 ml of diethyl ether three times. While the water layer was cooled, a 20% sodium hydroxide aqueous solution was added to make it alkaline, and the water layer was subjected to extraction with 50 ml of diethyl ether three times, and dried over 10 g of anhydrous sodium sulfate. Then, the solvent was distilled off under reduced pressure to give 1.48 g of 1-(3,5-dimethylphenoxy)-2-aminopropane (yield 83.7%).

WORKUP

后处理

  1. customthe reaction
  2. temperatureto cool
  3. washthe mixture was washed with 20 ml of diethyl ether three times
  4. temperatureWhile the water layer was cooled
  5. additiona 20% sodium hydroxide aqueous solution was added
  6. extractionthe water layer was subjected to extraction with 50 ml of diethyl ether three times
  7. dry with materialdried over 10 g of anhydrous sodium sulfate
  8. distillationThen, the solvent was distilled off under reduced pressure