HRID483814

反应详情

EQUATION

反应方程式

HRID 483814 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewas refluxed for 20 hours
  2. customevaporated down
  3. customthe residue was partitioned in H2O/methylene chloride
  4. customAfter the undissolved constituents had been separated off
  5. washthe organic phase was washed once with 1 N NaOH
  6. dry with materialwith H2O, dried over Na2SO4
  7. customevaporated down
  8. customthe residue was recrystallized from methanol
  9. customdried