Piperazine → 2-nitro-5-piperazin-1-yl-benzoic Acid

Participants

Reaction Conditions

Reaction Steps

5-Chloro-2-nitro-benzoic acid (44 g) and piperizine (90 g, 4.8 eq.) were mixed without solvent and heated at 110° C. for 6 hours and then stirred at room temperature over night. At this time, the mixture had solidified. To this solid was added 10% KHSO4 (wt/vol, pH 4 to 5) aqueous solution and the mixture was sonicated. The supernatant was decanted and fresh 10% KHSO4 (wt/vol) aqueous solution was added. A total of 1.8 liters of 10% KHSO4 (wt/vol) aqueous solution was added and decanted in this manner. After stirring at room temperature, the solid was filtered and rinsed with water. The remaining solid was dried in a vacuum oven, leaving a yellow-orange solid (53.1 g). This material was carried forward to the next step without further purification.

Provenance & Evidence