1,1,1-Triethoxybutane → 4-Chloro-1-propyl[1,2,4]triazolo[4,3-a]quinoxaline

HRID 464283

Reaktionsgleichung

Reaktionsgleichung von HRID 464283
[Cl:1][C:2]1[C:11]([NH:12][NH2:13])=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[C:14](OCC)(OCC)(OCC)[CH2:15][CH2:16][CH3:17]>>[Cl:1][C:2]1[C:11]2[N:10]([C:14]([CH2:15][CH2:16][CH3:17])=[N:13][N:12]=2)[C:9]2[C:4]([N:3]=1)=[CH:5][CH:6]=[CH:7][CH:8]=2

Komponenten

3

Edukt 2

HCID 3717791,1,1-TriethoxybutaneHCID 36588202-Chloro-3-hydrazinoquinoxaline

Produkt 1

HCID 133857074-Chloro-1-propyl[1,2,4]triazolo[4,3-a]quinoxalineAusbeute 53 %

Versuchsvorschrift

2-Chloro-3-hydrazinoquinoxaline (3.0 g., 0.015 mole), the product of Example 1, was stirred with triethyl orthobutyrate (27 ml.) at 100° C. for 2 hours. The mixture was cooled to room temperature, and the precipitate was collected by filtration and washed with cyclohexane. The crude solid was taken up in chloroform and filtered to remove insoluble material. The chloroform solution was concentrated in vacuo to give a solid which was recrystallized from chloroform to give 1.96 g. (53% yield) of 4-chloro-1-n-propyl-[1,2,4]triazolo[4,3-a]quinoxaline, m.p. 173°-175° C. Mass spectrum: m/e, 246 (P).

Aufarbeitung

  1. filtrationthe precipitate was collected by filtration
  2. washwashed with cyclohexane
  3. filtrationfiltered
  4. customto remove insoluble material
  5. concentrationThe chloroform solution was concentrated in vacuo
  6. customto give a solid which
  7. customwas recrystallized from chloroform
  8. customto give 1.96 g

Quellen und Nachweise

ORD-Eintrag
ord-7a0b78267b9a4824a891d14362ac4141
Quelldatensatz
uspto-grants-1985_10
Patentnummer
US04547501

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