Reaktion #86318

Reaktionsgleichung

HCl

6-methyl-5-(6-(trifluoromethyl)-1H-indazol-4-yl)picolinonitrile

sodium hydroxide

EtOH

→

title compound

Ausbeute 89.0%

6-methyl-5-(6-(trifluoromethyl)-1H-indazol-4-yl)picolinic acid

Ausbeute 89.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux
2. 2
   SonstigeVolatiles were evaporated
3. 3
   Sonstigethe residue purified by CombiFlash® chromatography (5-40% MeOH in DCM over 120 minutes)
4. 4
   Einengenconcentrated in vacuo

Vorschrift

To 6-methyl-5-(6-(trifluoromethyl)-1H-indazol-4-yl)picolinonitrile (1.7 g, 5.62 mmol) in EtOH (20 mL) was added sodium hydroxide (14.06 mL, 28.1 mmol) and the resulting mixture was stirred for 16 hours at reflux. The mixture was subsequently cooled to room temperature and acidified with concentrated HCl. Volatiles were evaporated and the residue purified by CombiFlash® chromatography (5-40% MeOH in DCM over 120 minutes). The product-containing fractions were combined and concentrated in vacuo to give the title compound as a white solid (1.6 g, 89%). ESI-MS m/z [M+H]+ calc'd for C15H10F3N3O2, 322.1. found 322.06.

Quelle