Acetic Acid → HCID 18549190, compound

Participants

Reaction Steps

While stirring under ice-cooling, 10% hexane solution of sulfuryl chloride (0.019 ml, 0.24 mmol) was added to acetic acid (3 ml) solution of 2-{2,5-bis(trifluoromethyl)phenyl}amino-3-ethyl-6-trifluoromethyl-4(3H)-pyrimidinone (0.10 g, 0.24 mmol), followed by stirring for 1.5 hours while gradually returning to room temperature. After completion of the reaction, ice-water (10 ml) and ether (10 ml) were added to the reaction solution to separate the organic layer, and the resulting aqueous layer was extracted with ether (10 ml×3). The organic layers were combined, washed with water (20 ml×2) and then dried over anhydrous magnesium sulfate. The drying agent was removed by filtration, and the resulting filtrate was concentrated under a reduced pressure. By recrystallizing the thus obtained crude product from chloroform/hexane, 2-{2,5-bis(trifluoromethyl)phenyl}amino-5-chloro-3-ethyl-6-trifluoromethyl-4(3H)-pyrimidinone [Compound No. 49] was obtained.

Provenance & Evidence