反应详情

温度

150 °C

Iodine (4.8 g, 18.91 mmol) and H3PO2 (5.1 mL of a 50% aqueous solution, 46.8 mmol) were added to a solution of (rac)-1-(6-chloro-imidazo[1,2-b]pyridazin-3-yl)-1-(imidazo[1,2-a]pyridin-6-yl)ethanol (Stage 292.1, 1.85 g, 5.90 mmol) in acetic acid (50 mL). The RM was portion wise in 3 different microwave reactors and was heated at 150° C. for 5 min under microwave irradiations. It was basified with 2.5 N NaOH solution and then it was extracted twice with EtOAc/MeOH (9:1) twice. Combined organic layers was washed with brine and dried over Na2SO4, filtered and concentrated to give the title compound as a brown solid (tR 0.5 min (conditions 2), MH+=298)

1. extractionit was extracted twice with EtOAc/MeOH (9:1) twice
2. washCombined organic layers was washed with brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated