HRID328881

反应详情

EQUATION

反应方程式

HRID 328881 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of 4.8 parts of 1-(tert.-butyl)-3-azetidinol, 6.1 parts of 2,3-xylenol and 1.4 parts of trifluoroacetic acid was heated at 130° C. for 12 hours. The reaction mixture was cooled and dissolved in 100 parts of ether, and the solution was washed three times with 50 parts of 2N-sodium hydroxide aqueous solution and extracted three times with 2N-hydrochloric acid aqueous solution. The extract was washed twice with 50 parts of ether and made alkaline by addition of 2N-sodium hydroxide solution. The extraction was conducted three times with 50 parts of ether, and the extract was condensed and distilled under reduced pressure to yield 3.2 parts of 1-(2',3'-dimethylphenyloxy)-3-(tert.-butylamino)-2-propanol having a melting point of 57° C. and a boiling point of 134°-136° C. under 0.7 mm Hg.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. washthe solution was washed three times with 50 parts of 2N-sodium hydroxide aqueous solution
  3. extractionextracted three times with 2N-hydrochloric acid aqueous solution
  4. washThe extract was washed twice with 50 parts of ether
  5. additionby addition of 2N-sodium hydroxide solution
  6. extractionThe extraction
  7. customcondensed
  8. distillationdistilled under reduced pressure