5-Chloro-2-nitrobenzoic acid → HCID 59238177, compound

Participants

Reaction Conditions

Reaction Steps

5-Chloro-2-nitro-benzoic acid (42.3 g) and homopiperizine (100 g, 4.8 eq.) were mixed without solvent and heated at 110° C. After 10 min, the mixture had melted into an orange, thick solution. After 45 min total reaction time, the mixture turned to a dark black-brown color and become very thick. At this time, the mixture was cooled to room temperature and diluted with 10% KHSO4 (wt/vol) aqueous solution (pH 4). This mixture was stirred at room temperature for ˜1 hour and then filtered. The solid was rinsed with a mixture of hexanes and diethyl ether, diethyl ether and then hexane. The solid was then dried under vacuum. This resulted in 40.8 g (73%) of a dark brown solid. The compound was carried on to the next step without further analysis or purification.

Provenance & Evidence