3-Amino-5-methyl-4H-1,2,4-triazole → HCID 178469337, Verbindung

HRID 973850

Reaktionsgleichung

Reaktionsgleichung von HRID 973850
[NH2:1][C:2]1[N:6]=[C:5]([CH3:7])[NH:4][N:3]=1.[C:8]([C:13]([O:15][CH2:16][CH3:17])=[O:14])#[C:9][C:10]([O-])=[O:11]>C(O)C>[CH2:16]([O:15][C:13]([C:8]1[CH:9]=[C:10]([OH:11])[N:6]2[C:5]([CH3:7])=[N:4][N:3]=[C:2]2[N:1]=1)=[O:14])[CH3:17]

Komponenten

4

Edukt 2

HCID 2346103-Amino-5-methyl-4H-1,2,4-triazoleHCID 713605754-Ethoxy-4-oxobut-2-ynoate

Produkt 1

HCID 178469337HCID 178469337, VerbindungAusbeute 32,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A suspension of 14.7 g of 3-amino-5-methyl-s-triazole and 26.8 g of ethyl acetylenedicarboxylate in 120 ml of ethanol was refluxed for three hours, the reaction mixture was allowed to stand at room temperature for one hour, and the formed crystals were collected by filtration. The filtrate was concentrated and the residue was recrystallized from dichloromethane, and the crystals were joined with those obtained above. Purification by silica gel chromatography gave 10.8 g of the objective compound as colorless crystals.

Aufarbeitung

  1. temperaturewas refluxed for three hours
  2. filtrationthe formed crystals were collected by filtration
  3. concentrationThe filtrate was concentrated
  4. customthe residue was recrystallized from dichloromethane
  5. customthose obtained above
  6. customPurification by silica gel chromatography

Quellen und Nachweise

ORD-Eintrag
ord-5371e796ddc745a7aca9b7704cf9d928
Quelldatensatz
uspto-grants-1991_11
Patentnummer
US05064953

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