HRID1605960

反应详情

EQUATION

反应方程式

HRID 1605960 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

0.2 g. of powdered iron is added to a solution of 0.34 g. of 4-(p-fluorophenyl)-1,2,3,6-tetrahydro-1-[2-(p-nitrophenoxy) ethyl]pyridine in a mixture of 2 ml. of 1N hydrochloric acid, 10 ml. of ethanol and 10 ml. of water. The mixture is refluxed for 4 hrs., cooled and made alkaline by addition of 1N sodium hydroxide. After addition of 20 ml. of chloroform and celite, the mixture is filtered. The organic phase is separated, dried and evaporated. The oily residue obtained is dissolved in ethyl acetate and converted to the hydrochloride by addition of ethanolic hydrogen chloride. The 1-[2-(p-aminophenoxy)ethyl]-4-(p-fluorophenyl)-1,2,3,6-tetrahydropyridine dihydrochloride obtained in this way has m.p. 180°-181° after recrystallization from ethanol/ethylacetate/ether.

WORKUP

后处理

  1. temperatureThe mixture is refluxed for 4 hrs
  2. temperature, cooled
  3. additionAfter addition of 20 ml
  4. filtrationof chloroform and celite, the mixture is filtered
  5. customThe organic phase is separated
  6. customdried
  7. customevaporated
  8. customThe oily residue obtained