HRID1706442

反应详情

EQUATION

反应方程式

HRID 1706442 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 294 g. of 6-fluoroquinoline, 74.6 g. of quinaldine, 1.7 l. of chlorobenzene and 254 g. of iodine is stirred for 2 hours at 20°-25° C., then stirred and heated at 100° C. for 4 days. About 1 l. of solvent is removed by evaporation at reduced pressure and the residue is cooled to 0°-5° C. The precipitate is collected, washed with cold chlorobenzene, dried and pulverized. The finely divided solid is suspended with stirring and cooling in 500 ml. of methanol and 55 ml. of hydrazine is added to destroy excess iodine. The resulting solid 3-fluoroimidazo[1,2-a:3,4-a']diquinolin-15-ium iodide is collected by filtration, washed with cold methanol and dried; m.p. 310°-316° C.

WORKUP

后处理

  1. additionA mixture of 294 g
  2. customof solvent is removed by evaporation at reduced pressure
  3. temperaturethe residue is cooled to 0°-5° C
  4. customThe precipitate is collected
  5. washwashed with cold chlorobenzene
  6. customdried
  7. stirringwith stirring
  8. temperaturecooling in 500 ml
  9. additionof hydrazine is added
  10. customto destroy excess iodine
  11. filtrationThe resulting solid 3-fluoroimidazo[1,2-a:3,4-a']diquinolin-15-ium iodide is collected by filtration
  12. washwashed with cold methanol
  13. customdried