Cyanuric chloride → 4,6-dichloro-2-ethoxycarbonylmethylamino-S-triazine

HRID 1757606

Reaktionsgleichung

Reaktionsgleichung von HRID 1757606
[N:1]1[C:8]([Cl:9])=[N:7][C:5](Cl)=[N:4][C:2]=1[Cl:3].Cl.[NH2:11][CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14].C(=O)(O)[O-].[Na+]>>[Cl:9][C:8]1[N:1]=[C:2]([Cl:3])[N:4]=[C:5]([NH:11][CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])[N:7]=1

Komponenten

4

Edukt 3

HCID 7954Cyanuric chlorideHCID 516892Sodium BicarbonateHCID 2723640Glycine ethyl ester, hydrochloride

Produkt 1

HCID 147462614,6-dichloro-2-ethoxycarbonylmethylamino-S-triazine

Versuchsvorschrift

36.9 g of cyanuric chloride, 27.9 g of ethyl glycinate hydrochloride and 33.6 g of sodium bicarbonate were heated under reflux in 200 ml of dioxanefor 30 minutes. At the end of this time, the dioxane was removed by distillation under reduced pressure, and a mixture of ethyl acetate and water was added to the resulting residue, after which the mixture was shaken. The ethyl acetate layer was separated, dried and concentrated by evaporation under reduced pressure, and the resulting residue was recrystallized from a mixture of hexane and ethyl acetate, to yield 45.0 gof the title compound as crystals melting at 82° to 87° C.

Aufarbeitung

  1. temperatureunder reflux in 200 ml of dioxanefor 30 minutes
  2. customAt the end of this time, the dioxane was removed by distillation under reduced pressure
  3. additiona mixture of ethyl acetate and water
  4. additionwas added to the resulting residue
  5. customThe ethyl acetate layer was separated
  6. customdried
  7. concentrationconcentrated by evaporation under reduced pressure
  8. customthe resulting residue was recrystallized from a mixture of hexane and ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-a263c55c9326424cab865273cb512687
Quelldatensatz
uspto-grants-1995_08
Patentnummer
US05446144

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