HRID328906

反应详情

EQUATION

反应方程式

HRID 328906 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of 21.8 g of p-aminophenol, 22 g of 1-(tert.-butyl)-3-azetidinol and 0.73 g of potassium hydroxide was heated under nitrogen gas at 140° C. for 8 hours with agitation. The reaction mixture was cooled and dissolved in concentrated hydrochloric acid and the solution was extracted with ether. The hydrochloric acid aqueous solution was made alkaline with 10% -NaOH aqueous solution and then extracted with ether. The ether solution was washed with water and dried over anhydrous sodium sulfate. Then ether was distilled off and the residue was recrystallized from benzene. As a result 8g of 1-(p-aminophenoxy)-3-(tert.-butylamino)-2-propanol melting at 125° - 127° C were obtained. The results of infra-red spectrum analysis and nuclear magnetic resonance analysis are as follows:

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. extractionthe solution was extracted with ether
  3. extractionextracted with ether
  4. washThe ether solution was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThen ether was distilled off
  7. customthe residue was recrystallized from benzene