反应详情

A solution of 6-chloroindazole (1-3, 5.24 g, 34.3 mmol) in ethanol (500 mL) was reacted at the ambient temperature with iodine (8.72 g, 34.3 mmol) in the presence of silver sulfate (10.7 g, 34.3 mmol). After 2 h stirring at the same temperature, all the precipitates were removed by filtration and the filtrate solution was concentrated in vacuo. Trituation with dichloromethane and hexanes gave the desired product as an orange solid (1-4); 1H NMR (400 MHz, DMSO-d6) δ 13.62 (bs, 1H), 7.66 (d, 1H, J=1.6 Hz), 7.46 (d, 1H, J=8.5 Hz), 7.21 (dd, 1H, J=8.6, 1.6 Hz).

1. customall the precipitates were removed by filtration
2. concentrationthe filtrate solution was concentrated in vacuo