1,3-Butanedione, 4,4,4-trifluoro-1-(3-pyridinyl)- → HCID 13309053, Verbindung

HRID 326093

Reaktionsgleichung

Reaktionsgleichung von HRID 326093
[NH2:1][C:2]1[N:6]=[C:5]([CH3:7])[NH:4][N:3]=1.[F:8][C:9]([F:22])([F:21])[C:10](=O)[CH2:11][C:12]([C:14]1[CH:15]=[N:16][CH:17]=[CH:18][CH:19]=1)=O>C(O)(=O)C>[CH3:7][C:5]1[N:6]=[C:2]2[N:1]=[C:10]([C:9]([F:22])([F:8])[F:21])[CH:11]=[C:12]([C:14]3[CH:15]=[N:16][CH:17]=[CH:18][CH:19]=3)[N:3]2[N:4]=1

Komponenten

4

Edukt 2

HCID 684951,3-Butanedione, 4,4,4-trifluoro-1-(3-pyridinyl)-HCID 2346103-Amino-5-methyl-4H-1,2,4-triazole

Produkt 1

HCID 13309053HCID 13309053, VerbindungAusbeute 47,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A reaction mixture of 0.986 g of 3-amino-5-methyl-1,2,4-triazole and 2.178 g of 4,4,4-trifluoro-1-(3-pyridyl)-1,3-butanedione in 25 ml of glacial acetic acid was refluxed for 4 hours. The mixture was then evaporated to dryness in vacuo and gave a crystalline residue. This residue was partitioned between a saturated aqueous sodium bicarbonate solution and dichloromethane and the procedure of Example 1 was continued to give 1.33 g of the desired product as colorless crystals, mp 195°-197° C.

Aufarbeitung

  1. temperaturewas refluxed for 4 hours
  2. customThe mixture was then evaporated to dryness in vacuo
  3. customgave a crystalline residue
  4. customThis residue was partitioned between a saturated aqueous sodium bicarbonate solution and dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-55b027c0f6054b40b6bacef41597db46
Quelldatensatz
uspto-grants-1984_04
Patentnummer
US04444774

Verknüpfte Notizen

Wird geladen…