Reaktion #306297

Reaktionsgleichung

(6-phenyl-[1,2,4]triazolo[4,3-b][1,2,4]triazin-3-yl)methanol

Reactant 2

(6-(1-isopropyl-1H-pyrazol-4-yl)-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methanamine hydrochloride

DBU

toluene

→

3-(azidomethyl)-6-phenyl-[1,2,4]triazolo[4,3-b][1,2,4]triazine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeflushed with argon
2. 2
   Sonstigesealed
3. 3
   EinengenThe dark maroon mixture was concentrated
4. 4
   Sonstigethe resulting dark purple/black oil was purified by column chromatography
5. 5
   Sonstigeover 20 minutes

Vorschrift

A 16 mm test tube was charged with (6-phenyl-[1,2,4]triazolo[4,3-b][1,2,4]triazin-3-yl)methanol (0.500 g, 2.20 mmol), Reactant 2 (0.951 ml, 4.40 mmol), DBU (0.663 ml, 4.40 mmol), and toluene (8.16 ml, 77.0 mmol), flushed with argon, sealed, then stirred at room temperature for 3 hours. The dark maroon mixture was concentrated and the resulting dark purple/black oil was purified by column chromatography using a gradient of 3-5% MeOH/DCM over 20 minutes. 3-(azidomethyl)-6-phenyl-[1,2,4]triazolo[4,3-b][1,2,4]triazine was isolated as a brown solid.

Quelle