HRID1706444

反应详情

EQUATION

反应方程式

HRID 1706444 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 88.3 g. of 6-fluoroquinoline, 27.8 g. of 6-(1-methylethyl)quinaldine and 76.2 g. of iodine in 100 ml. of toluene is heated at 95°-100° C. for 5 days, cooled and diluted with 350 ml. of ethyl acetate. The precipitate is collected, pulverized, suspended in 500 ml. of aqueous methanol and recovered by filtration. The solid is suspended in 400 ml. of cold methanol, stirred with 6 ml. of hydrazine and the solid 3-fluoro-10-(1-methylethyl)imidazo[1,2-a:3,4-a']diquinolin-15-ium iodide is collected by filtration; m.p. 305°-307° C., after crystallization from methanol.

WORKUP

后处理

  1. temperaturecooled
  2. additiondiluted with 350 ml
  3. customThe precipitate is collected
  4. filtrationof aqueous methanol and recovered by filtration
  5. filtrationof hydrazine and the solid 3-fluoro-10-(1-methylethyl)imidazo[1,2-a:3,4-a']diquinolin-15-ium iodide is collected by filtration
  6. customm.p. 305°-307° C., after crystallization from methanol