HRID358126

反应详情

EQUATION

反应方程式

HRID 358126 的结构方程式

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To 200 ml of acetone were added 10.0 g of D-xylose and 175 mg of hydriodic acid (57%) and the mixture was refluxed with stirring in a water bath at 60° C. for 5 hours. During this reaction, the refluxing solvent was dried with 20 g of Molecular Sieves 3A interposed between the reaction vessel and the cooling jacket. After completion of the reaction, a small amount of pyridine was added and the acetone was distilled off under reduced pressure. The residue was dissolved in benzene and the benzene solution was washed with aqueous sodium bicarbonate and water and dried over anhydrous magnesium sulfate. The benzene was distilled off under reduced pressure and the residue was further distilled under reduced pressure, whereby 12.8 g (83.6%) of 1,2:3,5-di-O-isopropylidene-α-D-xylofuranose was obtained as a fraction boiling at 94°-97° C./3 mmHg.

WORKUP

后处理

  1. temperaturethe mixture was refluxed
  2. customDuring this reaction
  3. dry with materialthe refluxing solvent was dried with 20 g of Molecular Sieves 3A
  4. customAfter completion of the reaction
  5. distillationthe acetone was distilled off under reduced pressure
  6. dissolutionThe residue was dissolved in benzene
  7. washthe benzene solution was washed with aqueous sodium bicarbonate and water
  8. dry with materialdried over anhydrous magnesium sulfate
  9. distillationThe benzene was distilled off under reduced pressure
  10. distillationthe residue was further distilled under reduced pressure