Practical enantiomeric synthetic routes to 1,5-diaryl pyrazole acids

ORGN 157

Jimmy T. Liang, JLiang4@PRDUS.JNJ.COM, Neelakandha Mani, and Todd Jones. Johnson & Johnson Pharmaceutical Research Institute, 3210 Merryfield Row, San Diego, CA 92121
Practical routes for the enantioselective synthesis of 1,5-diaryl pyrazole acids, selective cholecystokinin 1 (CCK1) receptor antagonists, have been developed. A feature common to two routes is an efficient, regioselective construction of the pyrazole nucleus by reacting an aryl hydrazine with a disubstituted acetylenic ketone. In our first synthetic route, the desired stereochemistry was obtained by utilizing SFC to separate our racemic acid. In our second generation route involving 4 steps, the desired S-enantiomer was obtained in high optical purity (>92% ee) by a kinetic resolution using enzyme-catalyzed hydrolysis of the racemic ester. In our third synthetic route involving 6 steps, the desired stereochemistry at the chiral center was generated at an early stage by an enantioselective enol-protonation strategy using inexpensive (S)-(-)-ethyl lactate. All three methods furnished optically pure (>99% ee) final product as its crystalline sodium salt.