Reaktion #41459

Reaktionsgleichung

3-(2-(2-fluoro-5-iodobenzylidene)hydrazinyl)benzoic acid

potassium tert. butoxide

HCl

→

crude title compound

Ausbeute 107.4%

3-(5-iodo-1H-indazol-1-yl)benzoic acid

Ausbeute 107.4%

Lösungsmittel

NMP

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter cooling
2. 2
   Extraktionextracted trice with EtOAc
3. 3
   WaschenThe combined organic phases were washed twice with water
4. 4
   SonstigeEvaporation of the organic phase

Vorschrift

3-(2-(2-fluoro-5-iodobenzylidene)hydrazinyl)benzoic acid (3.47 g, 9 mmol) and potassium tert. butoxide (2.3 g, 20.5 mmol) was stirred under argon atmosphere in NMP (45 mL) at 150° C. for 30 min. After cooling, the mixture was diluted with water (100 mL), acidified with aqueous HCl (1.7 M) and extracted trice with EtOAc. The combined organic phases were washed twice with water and then with brine. Evaporation of the organic phase afforded crude title compound (3.52 g, quant.) as a light brown, amorphous, gummy solid.

Quelle