HRID462419

反应详情

EQUATION

反应方程式

HRID 462419 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.4 g of 1,3-dimethyl-7-(6-bromohexyl)-xanthine are boiled overnight under reflux in 50 ml of glacial acetic acid to which 1 ml of acetic anhydride and 5 g of potassium acetate have been added. After evaporation of the solvent by distillation in vacuo the residue is dissolved in 50 ml of 5% sulfuric acid on the addition of 20 ml methanol. The solution is boiled under reflux for 1 hour. The mixture is extracted with chloroform. The chloroform phase is washed until it is neutral and concentrated in vacuo. 1,3-dimethyl-7-(6-hydroxyhexyl)-xanthine having a melting point of 80° C. is obtained in a yield of more than 90%.

WORKUP

后处理

  1. additionhave been added
  2. customAfter evaporation of the solvent
  3. distillationby distillation in vacuo the residue
  4. dissolutionis dissolved in 50 ml of 5% sulfuric acid on the addition of 20 ml methanol
  5. temperatureunder reflux for 1 hour
  6. extractionThe mixture is extracted with chloroform
  7. washThe chloroform phase is washed until it
  8. concentrationconcentrated in vacuo