HRID1278033
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- extractionbefore extracting with 400 ml of diethyl ether
- dry with materialdry the ether phase over sodium sulfate
- concentrationconcentrate it
- dissolutionDissolve
- customthus-obtained residue in 250 ml of ethanol
- filtrationThen filter off the catalyst
- customdistil off the solvent
- distillationbefore distilling the product under a high vacuum
- customto obtain