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Methacrylamide → Ethyl [(2-methylacryloyl)amino](oxo)acetate

HRID 1073657
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1073657
[C:1]([NH2:6])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:7](Cl)([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:8]>C1C=CC=CC=1>[C:7]([NH:6][C:1](=[O:5])[C:2]([CH3:4])=[CH2:3])([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:8]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 6595MethacrylamideHCID 20884Ethoxalyl chloride

Produkt 1

HCID 14298183Ethyl [(2-methylacryloyl)amino](oxo)acetateAusbeute 42,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

Into a reaction vessel equipped with a stirrer, a cooler, an nitrogen gas introducing inlet and a dropping funnel, benzene (288.5 ml) and methacrylamide (49.1 g; 0.577 mol) were charged, and the resulting mixture was heated with reflux. Refluxing and bubbling with nitrogen gas were continued, during which ethoxalyl chloride (78.5 g; 0.577 mol) was dropwise added thereto in 2.5 hours. After the dropwise addition was completed, refluxing was continued for 5 hours. The benzene was distilled off, hydroquinone (0.01 g) was added thereto, and distillation under reduced pressure was carried out to give N-ethoxalylmethacrylamide (45.8 g). Yield, 43%. B.P., 110-115° C./0.3 mmHg. Refractive index, 1.473.

Aufarbeitung

  1. customInto a reaction vessel equipped with a stirrer
  2. additiona cooler, an nitrogen gas introducing inlet and a dropping funnel
  3. temperaturethe resulting mixture was heated
  4. temperaturewith reflux
  5. temperatureRefluxing
  6. custombubbling with nitrogen gas
  7. additionwas dropwise added
  8. additionAfter the dropwise addition
  9. temperaturerefluxing
  10. waitwas continued for 5 hours
  11. distillationThe benzene was distilled off
  12. additionhydroquinone (0.01 g) was added
  13. distillationdistillation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-95395c1ff753489589c39cfe63252450
Quelldatensatz
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04970281

Notizen zur Reaktion

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