HRID362632

反应详情

EQUATION

反应方程式

HRID 362632 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

139.6 g (1 mole) of glycine ethyl ester hydrochloride was dissolved in 80 ml of distilled water and to this solution was added 230 ml of an aqueous solution of 67.3 g (1.2 mole eq.) of potassium hydroxide. Then, 106.2 g (2 mole eq.) of acrylonitrile was added to the reaction solution while heating and stirring at 50° to 60° C. The reaction mixture was stirred for 5 hours with heating and then the organic layer was separated. The aqueous layer was extracted with ethyl ether and the extract was combined with the organic layer as separated above. The combined organic layer was dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure to remove the solvent. The residue was distilled under reduced pressure (100° to 150° C./10.25 torr) to obtain 65.6 g (Yield: 48%) of the title compound.

WORKUP

后处理

  1. temperaturewhile heating
  2. stirringThe reaction mixture was stirred for 5 hours
  3. temperaturewith heating
  4. customthe organic layer was separated
  5. extractionThe aqueous layer was extracted with ethyl ether
  6. customas separated above
  7. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationThe filtrate was concentrated under reduced pressure
  10. customto remove the solvent
  11. distillationThe residue was distilled under reduced pressure (100° to 150° C./10.25 torr)