HRID849383

反应详情

EQUATION

反应方程式

HRID 849383 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

400 mg of diphenylmethyl methyl D-tartarate was dissolved in 7 ml of toluene, and a catalytic amount of Amberlyst 15 and 1 ml of triethyl orthoformate were added, followed by refluxing under heating for one hour. Amberlyst was filtered off. Then, the filtrate was extracted by an addition of water and ethyl acetate. The organic layer was washed with a saturated sodium hydrogen carbonate aqueous solution and a saturated sodium chloride aqueous solution and then, dried over anhydrous magnesium sulfate. The drying agent was filtered off, and then, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=5/1) to obtain 195 mg of the above identified compound as a colorless oily substance.

WORKUP

后处理

  1. temperatureby refluxing
  2. temperatureunder heating for one hour
  3. filtrationAmberlyst was filtered off
  4. extractionThen, the filtrate was extracted by an addition of water and ethyl acetate
  5. washThe organic layer was washed with a saturated sodium hydrogen carbonate aqueous solution
  6. dry with materiala saturated sodium chloride aqueous solution and then, dried over anhydrous magnesium sulfate
  7. filtrationThe drying agent was filtered off
  8. distillationthe solvent was distilled off under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=5/1)
  10. customto obtain 195 mg of the