HRID904294

反应详情

EQUATION

反应方程式

HRID 904294 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8.8 g. (0.05 mol) of 3-methyl-4-hydroxy-coumarin are solubilised in 200 ml. of methyl isobutyl ketone at 80° C., and then, at this temperature, there are added 8.3 g. (0.06 mol) of anhydrous potassium carbonate and 0.5 g. of potassium iodide. The mixture is left for 1 hour at 80° C. while stirring. In 1 hour, there is added a solution of 9.8 g. (0.065 mol) of 2-morpholino-2-chlorethane in 50 ml. of methyl isobutyl ketone. The substance is then refluxed for 8 hours, filtered while hot and evaporated under vacuum. The oil which is obtained is taken up under heat in 200 ml. of a 5% solution of sodium bicarbonate, whereafter it is cooled, and extracted with 3×100 ml of ether. It is dried over NaSO4 and then the ether is evaporated under vacuum. A brown oil is obtained which cannot be crystallised. Weight 10 g.; yield 67% (theoretical yield 14.9 g.).

WORKUP

后处理

  1. waitIn 1 hour
  2. additionthere is added a solution of 9.8 g
  3. temperatureThe substance is then refluxed for 8 hours
  4. filtrationfiltered while hot and
  5. customevaporated under vacuum
  6. customThe oil which is obtained
  7. temperatureunder heat in 200 ml
  8. extractionextracted with 3×100 ml of ether
  9. dry with materialIt is dried over NaSO4
  10. customthe ether is evaporated under vacuum
  11. customA brown oil is obtained which
  12. customcannot be crystallised