Lithium iodide → HCID 11561873, compound

Participants

Reaction Steps

A solution of Example 596A (420 mg, 0.9 mmol), and LiI (482 mg, 4 equiv.) in 9 mL of pyridine was reacted in two vials in a microwave at 150° C. for 35 minutes. After concentration, the crude product 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 NH4OAc over 12 minutes (15 minute run time) at a flow rate of 70 mL/min. in 36 mg (8%) yield. MS (ESI(+)) m/e 471 (M+H)+; MS (ESI(−)) m/e 469 (M−H)−; 1H NMR (400 MHz, DMSO-d6) δ 1.21 (t, J=6.72 Hz, 6H) 1.55 (m, 4H) 2.01 (s, 2H) 2.28 (q, J=6.11 Hz, 2H) 2.55 (s, 2H) 2.86 (s, 2H) 3.05 (m, 6H) 6.30 (m, 1H) 6.81 (m, 1H) 7.11 (d, J=8.31 Hz, 1H) 7.17 (d, J=15.89 Hz, 1H) 7.35 (m, 1H) 7.51 (t, J=6.97 Hz, 1H) 7.57 (m, 1H) 7.93 (m, 1H).

Provenance & Evidence