HRID1904903
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureis heated
- filtrationThe hot reaction mixture is filtered
- customthe filtrate is evaporated in vacuo
- dissolutionthe residue is dissolved in 200 ml of water
- additionby adding 10% hydrochloric acid
- filtrationthe precipitate is filtered by suction
- customcrystallized twice from water