Reaktion #166228

Reaktionsgleichung

6-fluoro-2-(2-fluoro-4-iodo-phenylamino)-4-methoxy-3-nitro-benzaldehyde

hydrazine hydrate

→

title compound

Ausbeute 64.0%

(2-Fluoro-4-iodo-phenyl)-(6-methoxy-5-nitro-1H-indazol-4-yl)-amine

Ausbeute 64.0%

Lösungsmittel

DME

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated at 50° C. for 3 hours
2. 2
   EinengenThe reaction mixture was concentrated in vacuo
3. 3
   workup.ADDITIONthe residue treated with water
4. 4
   Filtrationthe resultant solid precipitate collected by filtration
5. 5
   Sonstigeto give a red/orange solid
6. 6
   SonstigeThe solid was recrystallised from IMS

Vorschrift

A biphasic mixture of 6-fluoro-2-(2-fluoro-4-iodo-phenylamino)-4-methoxy-3-nitro-benzaldehyde (1.5 g, 3.46 mmol) in hydrazine hydrate (10 mL) and DME (10 mL) was stirred at room temperature for 4 hours, then heated at 50° C. for 3 hours. The reaction mixture was concentrated in vacuo, the residue treated with water and the resultant solid precipitate collected by filtration to give a red/orange solid. The solid was recrystallised from IMS to give the title compound as a yellow solid (956 mg, 64%). LCMS (Method B) RT=3.62 min, [M+H]+=429 [M−H]−=427.

Quelle