Lithium iodide → HCID 11561873, compound

Participants

Reaction Steps

A solution of Example 597A (310 mg, 0.6 mmol), and LiI (322 mg, 4 equiv.) in 6 mL of pyridine was reacted in two vials in a microwave at 150° C. for 35 minutes and concentrated. The concentrate was purified by preparative HPLC on a Waters Symmetry C8 column (40 mm×100 mm, 7 μm particle size) using a gradient of 10% to 95% acetonitrile/10 mM aqueous ammonium acetate over 12 minutes (15 minute run time) at a flow rate of 70 mL/min. The product was combined with a sample of Example 596B to provide 256 mg of a 5:4 mixture of Example 596B and Example 597B.

Provenance & Evidence