反应详情

In a microwave vial, (rac)-1-(6-chloro-imidazo[1,2-b]pyridazin-3-yl)-1-(3-methyl-3H-benzoimidazol-5-yl)-ethanol (Stage 185.3, 650 mg, 1.507 mmol) was dissolved in AcOH (15 mL) under Argon. Iodine (1.148 g, 4.52 mmol) and H3PO2 (1.233 mL of a 50% aqueous solution, 11.3 mmol) were added and the mixture was submitted to MW-irradiation at 150° C. for 10 min. The mixture was diluted with water. It was basified until pH 5 with NaOH 10 M and then saturated NaHCO3 sol. until pH 7-8. It was then extracted with EtOAc one time. The organic phase was washed with brine, dried over Na2SO4, filtered and evaporated. It was then dried under vacuum overnight to afford the title compound as a foam (tR 2.12 min (conditions 8), MH+=312).

1. extractionIt was then extracted with EtOAc one time
2. washThe organic phase was washed with brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. customevaporated
6. customIt was then dried under vacuum overnight