HRID1278033

反应详情

EQUATION

反应方程式

HRID 1278033 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Boil 40.6 g of 2-(α-ethoxycarbonyl-4-chlorobenzylidene)-1-isopropylpyrrolidine and 115 ml of conc. hydrochloric acid under reflux until evolution of carbon dioxide ceases. Alkalize the resulting reaction mixture with 250 ml of 6 N sodium hydroxide solution before extracting with 400 ml of diethyl ether, dry the ether phase over sodium sulfate and concentrate it. Dissolve thus-obtained residue in 250 ml of ethanol, and hydrogenate the resulting solution with platinum/hydrogen. Then filter off the catalyst and distil off the solvent before distilling the product under a high vacuum to obtain a yield [21.8 g (70% of theory)] of title compound and having a b.p. of 75° at 7·10-3 mm of Hg.

WORKUP

后处理

  1. extractionbefore extracting with 400 ml of diethyl ether
  2. dry with materialdry the ether phase over sodium sulfate
  3. concentrationconcentrate it
  4. dissolutionDissolve
  5. customthus-obtained residue in 250 ml of ethanol
  6. filtrationThen filter off the catalyst
  7. customdistil off the solvent
  8. distillationbefore distilling the product under a high vacuum
  9. customto obtain