Iodine → HCID 135890114, compound

Participants

Reaction Steps

The compound (1.69 g, 3.9 mmol) of example 1 was added into methanol (15 ml), and added with silver nitrate (0.66 g, 3.9 mol), and then with I2 grain (0.98 g, 3.9 mmol) under stirring. The reaction mixture was stirred at room temperature for 0.5 h, and TLC showed that the reaction was complete. The reaction mixture was filtered, and the filtrate was concentrated. The concentrate was washed with water, extracted with dichloromethane. The organic layer was washed with saturated saline, dried with anhydrous sodium sulfate, and concentrated. The residue was recrystallized from ethyl acetate to give a yellowish solid (1.52 g, yield: 70%). 1H NMR (CDCl3) δ: 8.90 (1H, d), 7.89 (1H, dd), 7.16 (1H, d), 4.27 (2H, t), 3.46 (1H, m), 3.08 (4H, t), 2.49 (4H, t), 2.27 (3H, s), 2.03 (2H, m), 1.25 (6H, d), 1.16 (3H, t).

Provenance & Evidence