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Ethanol → Ethyl 2-dimethylaminomethylacrylate

HRID 616434
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 616434
[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]
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Komponenten

4

Edukt 2

HCID 702EthanolHCID 2235812-((Dimethylamino)methyl)prop-2-enoic acid

Produkt 1

HCID 20370247Ethyl 2-dimethylaminomethylacrylateAusbeute 55 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

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).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-0f51147892774f83bb0e5aca47167dc0
Quelldatensatz
uspto-grants-1978_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04074051

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