Ethyl 3-(methylamino)propanoate → HCID 21448613, Verbindung

HRID 596870Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 596870
[CH2:1]([O:3][C:4](=[O:9])[CH2:5][CH2:6][NH:7][CH3:8])[CH3:2].Cl[C:11]([C:13]([CH3:20])([CH3:19])[C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:12]>N1C=CC=CC=1>[O:12]=[C:11]([N:7]([CH3:8])[CH2:6][CH2:5][C:4]([O:3][CH2:1][CH3:2])=[O:9])[C:13]([CH3:20])([CH3:19])[C:14]([O:16][CH2:17][CH3:18])=[O:15]

Komponenten

4

Edukt 2

HCID 541480Ethyl 3-(methylamino)propanoateHCID 10559245Ethyl 3-chloro-2,2-dimethyl-3-oxopropanoate

Produkt 1

HCID 21448613HCID 21448613, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

To a solution of 61 g of N-methyl-β-alanine ethyl ester in 600 ml of dry pyridine there is added 82 g of ethyl 2-chloroformyl-2-methylpropionate. During the addition, which takes 30 minutes, the mixture is mechanically stirred and cooled with ice. Stirring is continued at 10° C for 30 minutes and then at 30° - 40° C for 1 hour. Next the pyridine is evaporated in vacuo, leaving a residue to which a small quantity of water is added, whereafter the mixture is extracted with ether. The extract is dried over magnesium sulphate and evaporated leaving the above-mentioned product as a liquid which is purified by distillation at reduced pressure. Yield 97 g (75%). Boiling point 134° - 136° C (1 mm). nD22 1.4565.

Aufarbeitung

  1. additionDuring the addition, which
  2. temperaturecooled with ice
  3. stirringStirring
  4. waitis continued at 10° C for 30 minutes
  5. waitat 30° - 40° C for 1 hour
  6. customNext the pyridine is evaporated in vacuo
  7. customleaving a residue to which a small quantity of water
  8. additionis added, whereafter the mixture
  9. extractionis extracted with ether
  10. dry with materialThe extract is dried over magnesium sulphate
  11. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-148b5c0942b0443ca46c1bfff9749119
Quelldatensatz
uspto-grants-1977_03
Patentnummer
US04012392

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