HRID5621

反应详情

EQUATION

反应方程式

HRID 5621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 206.7 g of methyl (R)-3-hydroxytetradecanoate in 1000 ml of cyclohexane was treated under nitrogen and while stirring with 214.2 g of benzyl trichloroacetimidate and dissolved at 20°. 10 ml of trifluoromethanesulphonic acid were added dropwise while cooling in an ice/water bath in such a manner that the temperature remains between 20°-23°. The resulting suspension was stirred at 25°-30°. The precipitate was filtered off, the filter cake was washed with cyclohexane, the filtrates were extracted with sat. NaHCO3 solution, water and sat. NaCl solution. The organic phase was dried over magnesium sulphate, filtered, the filter cake was washed with cyclohexane and the filtrates were evaporated. 314.5 g of methyl (R)-3-(benzyloxy)-tetradecanoate were obtained.

WORKUP

后处理

  1. additionwas treated under nitrogen
  2. dissolutiondissolved at 20°
  3. temperaturewhile cooling in an ice/water bath in such a manner that the temperature
  4. customremains between 20°-23°
  5. filtrationThe precipitate was filtered off
  6. washthe filter cake was washed with cyclohexane
  7. extractionthe filtrates were extracted with sat. NaHCO3 solution, water and sat. NaCl solution
  8. dry with materialThe organic phase was dried over magnesium sulphate
  9. filtrationfiltered
  10. washthe filter cake was washed with cyclohexane
  11. customthe filtrates were evaporated