Ethanol → Ethyl 2-dimethylaminomethylacrylate
反応式
[CH3:1][N:2]([CH2:4][C:5](=[CH2:9])[C:6]([OH:8])=[O:7])[CH3:3].[CH2:10](O)[CH3:11]>S(=O)(=O)(O)O>[CH3:1][N:2]([CH2:4][C:5](=[CH2:9])[C:6]([O:8][CH2:10][CH3:11])=[O:7])[CH3:3]参加物
4
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-0f51147892774f83bb0e5aca47167dc0
- 出典データセット
- uspto-grants-1978_02
- 特許番号
- US04074051
反応ノート
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