Ethyl orthoformate → 8-(3-Pyridinyl)-1,2,4-triazolo[4,3-a]pyridine

HRID 465115Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 465115
[NH:1]([C:3]1[C:8]([C:9]2[CH:10]=[N:11][CH:12]=[CH:13][CH:14]=2)=[CH:7][CH:6]=[CH:5][N:4]=1)[NH2:2].[CH:15](OCC)(OCC)OCC>>[N:11]1[CH:12]=[CH:13][CH:14]=[C:9]([C:8]2[C:3]3[N:4]([CH:15]=[N:2][N:1]=3)[CH:5]=[CH:6][CH:7]=2)[CH:10]=1

Komponenten

3

Edukt 2

HCID 31214Ethyl orthoformateHCID 135337152-Hydrazino-3,3'-bipyridine

Produkt 1

HCID 135337048-(3-Pyridinyl)-1,2,4-triazolo[4,3-a]pyridine

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A 4.15 g portion of 2-hydrazino-3,3'-bipyridine was dissolved in 30 ml of triethyl orthoformate and heated at 100° C. for 2 hours. The volatiles were removed at reduced pressure and the residue purified by chromatography on hydrous magnesium silicate, eluting with ethyl acetate. The solid was recrystallized from methylene chloride-hexane, giving 2.67 g of the desired product, mp 186°-189° C.

Aufarbeitung

  1. customThe volatiles were removed at reduced pressure
  2. customthe residue purified by chromatography on hydrous magnesium silicate
  3. washeluting with ethyl acetate
  4. customThe solid was recrystallized from methylene chloride-hexane

Quellen und Nachweise

ORD-Eintrag
ord-db9af6fd3a9f4d898db18d8f8c613664
Quelldatensatz
uspto-grants-1985_10
Patentnummer
US04550166

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