HRID616434

反应详情

EQUATION

反应方程式

HRID 616434 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-dimethylaminomethylacrylic acid (129g) in concentrated sulphuric acid (105 ml, 98%) and ethanol (500 ml) was boiled under reflux for 3 hours. After evaporating to half volume and pouring the residue into water (1 liter), anhydrous sodium carbonate (212g) was added and the solution was allowed to stand for 3 hours, when it gave a neutral reaction. The aqueous mixture was extracted with ether (3 × 250 ml), after drying over anhydrous sodium sulphate, the ether extract was evaporated at atmospheric pressure. The residual pale yellow oil was distilled under reduced pressure to give ethyl 2-dimethylaminomethylacrylate (86g, 55% boiling point 84° C/20 mm).

WORKUP

后处理

  1. temperatureunder reflux for 3 hours
  2. customAfter evaporating to half volume
  3. additionpouring the residue into water (1 liter), anhydrous sodium carbonate (212g)
  4. additionwas added
  5. customwhen it gave
  6. customa neutral reaction
  7. extractionThe aqueous mixture was extracted with ether (3 × 250 ml)
  8. dry with materialafter drying over anhydrous sodium sulphate
  9. extractionthe ether extract
  10. customwas evaporated at atmospheric pressure
  11. distillationThe residual pale yellow oil was distilled under reduced pressure