HRID477581

反应详情

EQUATION

反应方程式

HRID 477581 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 20 ml of ethyl acetate was dissolved 0.73 g of 2,3,4-tri-O-acetyl-1-azido-1-deoxy-β-D-xylopyranose, and 65 mg of 10% Pd/C was added to the solution. Then the solution was stirred in a hydrogen atmosphere for 2 hours. The Pd/C was removed by filtration, and the filtrate was concentrated. To the concentrate was added 20 ml of pyridine, 3 ml of acetic anhydride and then 10 mg of 4-dimethylaminopyridine, and the mixture was stirred for 16 hours. Water was added to the reaction, and the mixture was extracted with chloroform. The chloroform layer was washed with 0.1 N HCl solution, 1% sodium bicarbonate solution and finally with water, dehydrated and concentrated. The residue was subjected to silica gel column chromatography with a system of chloroform-acetone (100:1) to obtain 0.4 mg of 1-acetamido-2,3,4-tri-O-acetyl-1-deoxy-β-D-xylopyranose.

WORKUP

后处理

  1. additionwas added to the solution
  2. customThe Pd/C was removed by filtration
  3. concentrationthe filtrate was concentrated
  4. additionTo the concentrate was added 20 ml of pyridine, 3 ml of acetic anhydride
  5. additionWater was added to the reaction
  6. extractionthe mixture was extracted with chloroform
  7. washThe chloroform layer was washed with 0.1 N HCl solution, 1% sodium bicarbonate solution and finally with water
  8. concentrationconcentrated