Reaktion #68492

ord-9906acc1e70341139e36a3119039e418

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigesealed
  2. 2
    EinengenThe reaction mixture was concentrated
  3. 3
    Sonstigethe yellow residue was purified by MPLC
  4. 4
    Wascheneluting with a gradient of 3-8% MeOH/DCM over 80 minutes

Vorschrift

A 15 mL tube was charged with (6-phenyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methanamine (0.100 g, 0.444 mmol), 6-chloropurine (0.103 g, 0.666 mmol), and sec-butanol (3.00 ml, 32.4 mmol), sealed, then heated in a 100° C. oil bath for 5 hours. The reaction mixture was concentrated and the yellow residue was purified by MPLC using a 40 g RediSep column, eluting with a gradient of 3-8% MeOH/DCM over 80 minutes. N-((6-phenyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methyl)-7H-purin-6-amine (0.0500 g, 32.8% yield) was isolated as the hydrochloride salt.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524900B2uspto-grants-2013_09