HRID1278050

反应详情

EQUATION

反应方程式

HRID 1278050 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dissolve 27.9 g of 2-benzyl-1-methylpyrrolidine in 130 ml of conc. sulfuric acid, and add 100 ml of conc. nitric acid dropwise at 0°, with stirring, to the resulting solution. Continue stirring for a further 30 minutes at room temperature. Pour the mixture into 1 liter of ice water and alkalize with sodium hydroxide solution, with cooling. Extract the thus-produced preparation 4 times with, in each case, 150 ml of diethyl ether. Dry the ether phase over sodium sulfate and concentrate it to a red oil to obtain the title compound at a yield of 33.8 g (96% of theory). The hydrogen fumarate (from isopropanol) melts at 145° to 146°.

WORKUP

后处理

  1. stirringContinue stirring for a further 30 minutes at room temperature
  2. temperaturewith cooling
  3. extractionExtract
  4. customthe thus-produced preparation 4 times with, in each case, 150 ml of diethyl ether
  5. dry with materialDry the ether phase over sodium sulfate
  6. concentrationconcentrate it to a red oil