Reaktion #160603

Reaktionsgleichung

(2-fluoro-4-iodo-phenyl)-(2,3,5-trifluoro-6-nitro-phenyl)-amine

ammonium chloride

EtOAc

→

solid

Ausbeute 66.4%

3,4,6-Trifluoro-N2-(2-Fluoro-4-iodo-phenyl)-benzene-1,2-diamine

Ausbeute 66.4%

Lösungsmittel

EtOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux for 16 hours
2. 2
   SonstigeReaction mixture
3. 3
   Temperaturto cool
4. 4
   Filtrationwas filtered over celite and
5. 5
   Einengenconcentrated to dryness
6. 6
   SonstigeThe residue obtained
7. 7
   Waschenwas washed with water
8. 8
   TrocknenThe EtOAc layer was dried over sodium sulfate
9. 9
   Sonstigefurther purified by crystallization from EtOH

Vorschrift

To the stirred solution of (2-fluoro-4-iodo-phenyl)-(2,3,5-trifluoro-6-nitro-phenyl)-amine 3 (5.2 gm, 12.62 mmol) in EtOH (200 ml), ammonium chloride (10.12 gm, 189.3 mmol) and iron powder (10.57 gm, 189.3 mmol) was added. This reaction mixture was kept stirring at reflux for 16 hours. Reaction mixture was allowed to cool and was filtered over celite and concentrated to dryness. The residue obtained was taken into EtOAc and was washed with water. The EtOAc layer was dried over sodium sulfate and further purified by crystallization from EtOH to provide off-white solid (3.2 gm, yield: 66.39%). M−H+: 381.1. 1H NMR (DMSO, 300 MHz): 5.0 (s, 2H); 6.2 (t, 1H); 7.2-7.3 (m, 2H); 7.45 (s, 1H); 7.5 (d, 1H).

Quelle