HRID1904903

反应详情

EQUATION

反应方程式

HRID 1904903 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of a sodium ethylate solution prepared from 6.76 g of metallic sodium and 290 ml of anhydrous ethanol, 35 g of 2-(3-methyl-xanthine-7-yl)-acetamidoxime and 43.0 g of ethyl acetate is heated to boiling under stirring for 4 hours. The hot reaction mixture is filtered, the filtrate is evaporated in vacuo and the residue is dissolved in 200 ml of water. The pH of the solution is adjusted to 7 by adding 10% hydrochloric acid, the precipitate is filtered by suction and crystallized twice from water. Thus, 18.0 g of 3,7-dihydro-3-methyl-7-([5-methyl-1,2,4-oxadiazole-3-yl]-methyl)-1H-purine-2,6-dione are obtained, m.p.: 262°-264° C.

WORKUP

后处理

  1. temperatureis heated
  2. filtrationThe hot reaction mixture is filtered
  3. customthe filtrate is evaporated in vacuo
  4. dissolutionthe residue is dissolved in 200 ml of water
  5. additionby adding 10% hydrochloric acid
  6. filtrationthe precipitate is filtered by suction
  7. customcrystallized twice from water