Water → 5-Methyl-7-phenyl[1,2,4]triazolo[1,5-a]pyrimidin-2-amine

HRID 653573

Reaktionsgleichung

Reaktionsgleichung von HRID 653573
[NH2:1][C:2]1[N:6]=[C:5]([NH2:7])[NH:4][N:3]=1.[C:8]([CH2:16][C:17](=O)[CH3:18])(=O)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.C(Cl)Cl.O>C(O)(=O)C>[CH3:18][C:17]1[CH:16]=[C:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:3]2[N:4]=[C:5]([NH2:7])[N:6]=[C:2]2[N:1]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 6344DichloromethaneHCID 7166BenzoylacetoneHCID 150783,5-Diamino-1,2,4-triazole

Produkt 1

HCID 9757135-Methyl-7-phenyl[1,2,4]triazolo[1,5-a]pyrimidin-2-amineAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A mixture of 7.0 g (71 mmol) 3,5-diamino-1,2,4-triazole and 12.0 g (74 mmol) benzoylacetone in 100 ml of glacial acetic acid was heated at reflux 2 hours. After cooling, methylene chloride (200 ml) was added followed by the addition of excess water. The organic layer was separated, washed with water, brine, dried over magensium sulfate and evaporated in vacuo to give a solid residue to which ethyl acetate was added. Filtering gave 16.0 g of crude 5-methyl-7-phenyl-1,2,4-triazolo[1,5-a]pyrimidin-2-amine (m.p. 246°-250° C.) which was used directly in the next step.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux 2 hours
  3. temperatureAfter cooling
  4. customThe organic layer was separated
  5. washwashed with water, brine
  6. dry with materialdried over magensium sulfate
  7. customevaporated in vacuo
  8. customto give a solid residue to which ethyl acetate
  9. additionwas added
  10. filtrationFiltering

Quellen und Nachweise

ORD-Eintrag
ord-d978f1943c9f42c9a878a6ac2d50f561
Quelldatensatz
uspto-grants-1992_07
Patentnummer
US05127936

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