Reaktion #1161391

Reaktionsgleichung

product

2-[(3-Chloro-6-nitrophenyl)thio]-1-methyl-1H-imidazole

→

4-Chloro-2-[(1-methyl-1H-imidazol-2-yl)thio]benzenamine

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAIThydrogenation continued for 90 minutes
2. 2
   FiltrationThe mixture was filtered
3. 3
   Sonstigeto remove the catalyst
4. 4
   Einengenthe filtrates concentrated
5. 5
   SonstigeThe residue was recrystallized from dichloromethane/petroleum ether (bp 30°-60° C.)
6. 6
   Sonstigeto give the product as colorless plates (1.7 g, 66%), mp 116°-120° C.

Vorschrift

A mixture of 3.0 g (10.7 mmoles) of the product from Example 49, 1.5 spatulas of Raney nickel and 200 ml of ethanol was hydrogenated at 1 atmosphere and room temperature for 18 hours. An additional spatula of Raney nickel was added and hydrogenation continued for 90 minutes. The mixture was filtered to remove the catalyst and the filtrates concentrated. The residue was recrystallized from dichloromethane/petroleum ether (bp 30°-60° C.) to give the product as colorless plates (1.7 g, 66%), mp 116°-120° C.

Quelle