Methoxyacetic Acid → HCID 178494711, Verbindung

HRID 519501Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 519501
[CH3:1][O:2][CH2:3][C:4](O)=O.S(O)(O)(=O)=O.[NH2:12][NH:13][C:14]([NH2:16])=[NH:15].C(=O)([O-])O.[Na+]>ClC1C=CC(Cl)=CC=1Cl>[CH3:1][O:2][CH2:3][C:4]1[NH:15][C:14]([NH2:16])=[N:13][N:12]=1

Komponenten

5

Edukt 3

HCID 12251Methoxyacetic AcidHCID 516892Sodium BicarbonateHCID 178513188HCID 178513188, Verbindung

Produkt 1

HCID 178494711HCID 178494711, VerbindungAusbeute 96 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 131,2,4-TrichlorobenzeneLösungsmittel

Reaktionsbedingungen

Temperatur
200 °C

Versuchsvorschrift

A mixture of methoxyacetic acid (15 g), aminoguanidine sulfate (21 g) and 1,2,4-trichlorobenzene (20 mL) was stirred at 200° C. for 24 hr. The reaction mixture was poured into saturated aqueous sodium hydrogen carbonate, and the mixture was extracted with n-butanol. The obtained n-butanol layer was concentrated, and the residue was purified by silica gel column chromatography to give the title compound as a colorless solid (15 g, 75%).

Aufarbeitung

  1. extractionthe mixture was extracted with n-butanol
  2. concentrationThe obtained n-butanol layer was concentrated
  3. customthe residue was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-450ed2df79ef4a4cb2ace8cf372526bf
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09115136B2

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