HRID483814
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 5.0 g of 7-hydroxy-3,4-dimethylcoumarin, 3.9 g of 2-chloromethyl-5-methyl-1,3,4-thiadiazole, 3.5 g of K2CO3 and 100 ml of acetone was refluxed for 20 hours and evaporated down, and the residue was partitioned in H2O/methylene chloride. After the undissolved constituents had been separated off, the organic phase was washed once with 1 N NaOH and then with H2O, dried over Na2SO4 and evaporated down, and the residue was recrystallized from methanol and dried.
WORKUP
后处理
- temperaturewas refluxed for 20 hours
- customevaporated down
- customthe residue was partitioned in H2O/methylene chloride
- customAfter the undissolved constituents had been separated off
- washthe organic phase was washed once with 1 N NaOH
- dry with materialwith H2O, dried over Na2SO4
- customevaporated down
- customthe residue was recrystallized from methanol
- customdried