HRID616434
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
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
- temperatureunder reflux for 3 hours
- customAfter evaporating to half volume
- additionpouring the residue into water (1 liter), anhydrous sodium carbonate (212g)
- additionwas added
- customwhen it gave
- customa neutral reaction
- extractionThe aqueous mixture was extracted with ether (3 × 250 ml)
- dry with materialafter drying over anhydrous sodium sulphate
- extractionthe ether extract
- customwas evaporated at atmospheric pressure
- distillationThe residual pale yellow oil was distilled under reduced pressure