HRID1085683

反应详情

EQUATION

反应方程式

HRID 1085683 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 26 parts of (S)-4-[(4-fluorophenoxy)methyl]-2,2-dimethyl-1,3-dioxolane, 35 parts of a hydrochloric acid solution 2N and 80 parts of 2-propanone was stirred for 2 hours at reflux temperature. The mixture was stirred overnight at room temperature, diluted with 240 parts of ethanol and evaporated. The residue was dissolved in trichloromethane. The organic layer was washed twice with water, dried, filtered and evaporated. The residue was crystallized from tetrachloromethane. The product was filtered off and dried, yielding 11 parts (50.4%) of (-)-(R)-3-(4-fluorophenoxy)-1,2-propanediol; [α]D =-10.08° (c=0.5% in methanol) (146).

WORKUP

后处理

  1. temperatureat reflux temperature
  2. stirringThe mixture was stirred overnight at room temperature
  3. customevaporated
  4. dissolutionThe residue was dissolved in trichloromethane
  5. washThe organic layer was washed twice with water
  6. customdried
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue was crystallized from tetrachloromethane
  10. filtrationThe product was filtered off
  11. customdried