HRID542931

反应详情

EQUATION

反应方程式

HRID 542931 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.0 g of 2-trichloromethyl-8-methyl-4-chloro-quinoline are dissolved in 45 ml of dry dichloromethane and under intense stirring 1.5 ml of antimony-penta-chloride and 1.0 ml of antimony-penta-fluoride are added by dropping at a temperature of -5° to 0° C. The mixture is stirred at this temperature for 4 hours and allowed to stand at room temperature for 48 hours. 6 ml of icy concentrated hydrochloric acid are added, the precipitate is filtered, washed with some dichloromethane, the filtrate is separated, dried, filtered and evaporated. 2.1 g solid product are obtained which is recrystallized from heptane: 1.9 g of a yellowish crystalline substance, 68.2%, m.p.: 90°-94° C.

WORKUP

后处理

  1. additionare added
  2. customby dropping at a temperature of -5° to 0° C
  3. waitto stand at room temperature for 48 hours
  4. filtrationthe precipitate is filtered
  5. washwashed with some dichloromethane
  6. customthe filtrate is separated
  7. customdried
  8. filtrationfiltered
  9. customevaporated