HRID35934

反应详情

EQUATION

反应方程式

HRID 35934 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 4.00 g (105 mmol.) of lithium aluminum hydride and 50 ml of anhydrous tetrahydrofuran, there was added dropwise a solution of 2.50 g (10.5 mmol.) of 2-amino-3-[4-(1,1-dimethylethyl)phenoxy]propionic acid obtained in Production Example 13 in 50 ml of anhydrous tetrahydrofuran with stirring under reflux by heating for 30 minutes. Then the reaction mixture was further refluxed by heating with stirring for 2 hours. After the reaction was completed, the resultant mixture was cooled to a temperature of from 5° C. to 10° C. To the resultant mixture, there was added 100 ml of toluene and further added slowly, 10 ml of water and a 5N aqueous solution of sodium hydroxide. The above mixture was dried over anhydrous magnesium sulfate, filtrated with a filter agent (Celite®) and concentrated under reduced pressure to give 2.10 g of 2-amino-3-[4-(1,1-dimethylethyl)phenoxy]propanol as a light-yellowish solid (m.p. 101.7° C.).

WORKUP

后处理

  1. temperatureunder reflux
  2. temperatureby heating for 30 minutes
  3. temperatureThen the reaction mixture was further refluxed
  4. temperatureby heating
  5. stirringwith stirring for 2 hours
  6. additionfurther added slowly
  7. dry with materialThe above mixture was dried over anhydrous magnesium sulfate
  8. filtrationfiltrated with a filter agent (Celite®)
  9. concentrationconcentrated under reduced pressure