Potassium Carbonate → HCID 86689286, compound

Participants

Reaction Steps

To a mixture of 55 (2.08 g, 0.01 mol) and K2CO3 (3.45 g, 0.025 mol) in CH3CN (25 mL) was added a solution of 56a (2.46 g, 0.012 mol) in CH3CN (25 mL) over 45 min at rt under Ar. After stirring at rt for 3 hr, EtOAc (100 mL) and saturated NaHCO3 (100 mL) where added. The resulting mixture was stirred at rt for 10 min. The organic phase was washed with saturated NaHCO3 (1×75 mL) and brine (1×100 mL), filtered through phase separation filter paper, and concentrated in vacuo to give a solid. The solid was triturated with hexanes (100 mL), filtered, and dried to give 3.5 g (93%) of 58a as a purple solid. HPLC analysis showed a purity of 91%. 1H NMR (60 MHz, CDCl3): δ 7.6 (brs, 1H), 7.3-6.7 (m, 5H), 6.2 (m, 2H), 4.6 (s, 2H), 4.0 (q, 2H), 3.6 (brs, 1H), 2.8 (brs, 2H), 2.0-1.6 (m, 1H), 1.4 (t, 3H), 1.0 (d, 6H) ppm.

Provenance & Evidence