HRID1460985
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 1N 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 1N NaOH
- dry with materialwith H2O, dried over Na2SO4
- customevaporated down
- customthe residue was recrystallized from methanol
- customdried