Water → HCID 69000022, compound

Participants

Reaction Conditions

Reaction Steps

A suspension of 5-Methyl-2-(2′,4′-dichloro-3′-methylanilino)phenylacetic acid (15.42 mmoles) in acetone is heated to reflux temperature and allow to stir for 10 min at ca. 55° C. The resulting solution is slightly cooled to 50° C. and filtered hot over Whatman glasfiber filter. The filter is washed with acetone at 50° C. The filtrate is heated to 50° C. and a mixture of potassium hydroxide 45% (14.65 mmoles) (0.95 eq.) and water is dropwise added over ca. 15 min. The dropping funnel is rinsed with water and acetone. The resulting suspension is stirred at 50° C. for 30 min. The slurry is then allowed to cool to 25° C. over ca. 2 hours. The suspension is stirred over night at room temperature and filtered. The filter cake is washed in three portions. The crystals are dried first for 3 h at 50° C./10 mbar and then further for 17 h at 80° C./10 mbar to yield a white powder, m.p. 315-317° C., 326.9° C., melting enthalpy 29 J/g.

Provenance & Evidence