反应详情

Iodine (723 mg, 2.85 mmol) and H3PO2 (0.777 mL, 14.25 mmol) were added to a solution of (rac)-1-(5,7-difluoro-quinolin-6-yl)-1-[6-(1-methyl-1H-pyrazol-4-yl)-imidazo[1,2-b]pyridazin-3-yl]-ethanol (Stage 191.1, 386 mg, 0.950 mmol) in acetic acid (8 mL). The RM was subjected to MW-irradiation at 150° C. for 5 min. The RM was neutralized with 2.5 M NaOH solution and extracted twice with EtOAc. The organics were joined and washed with brine, then dried over Na2SO4 and the solvent was removed. The residue was triturated with Et2O and the precipitate was filtered off to afford the title compound a yellow solid (tR 0.95 min (conditions 2), MH+=391, 1H-NMR in DMSO-d6: 8.90 (d, 1H); 8.49 (d, 1H); 8.18 (s, 1H); 8.04 (d, 1H); 7.81 (s, 1H); 7.67 (d, 1H); 7.56 (dd, 1H); 7.42 (d, 1H); 5.10 (q, 1H); 3.85 (s, 3H); 1.91 (d, 3H)).

1. extractionextracted twice with EtOAc
2. washwashed with brine
3. dry with materialdried over Na2SO4
4. customthe solvent was removed
5. customThe residue was triturated with Et2O
6. filtrationthe precipitate was filtered off