反应详情

(rac)-1-(6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-1-(6-fluoro-1-methyl-1H-indazol-5-yl)-ethanol ((i), 21.4 g, 61.9 mmol) was dissolved in acetic acid (310 mL) and introduced in 20 microwave reactor-vials. Iodide (2.36 g×20, 186 mmol), followed by H3PO2 50% (2.56 mL×20, 464 mmol) were then added into each vial. Then they were submitted to microwave irradiations 10 min at 150° C. The combined RMs were concentrated in vacuo and the residue was diluted with water, basified by a 4 M NaOH solution and extracted twice with EtOAc. The organics were joined and washed with brine, dried over Na2SO4 and the solvent was removed. The residue was triturated with diisopropyl ether. The precipitate formed was filtered off to give a beige solid (tR 4.08 min (conditions 1), tR 14.39/16.40 min (conditions 2), MH+=330, 1H-NMR in DMSO-d6: 8.19 (d, 1H); 7.92 (s, 1H); 7.80 (s, 1H); 7.55 (d, 1H); 7.42 (d, 1H); 7.28 (d, 1H); 4.84 (m, 1H); 3.96 (s, 3H); 1.71 (d, 3H)).

1. additionintroduced in 20 microwave reactor-vials
2. additionwere then added into each vial
3. customirradiations 10 min
4. customat 150° C
5. concentrationThe combined RMs were concentrated in vacuo
6. additionthe residue was diluted with water
7. extractionextracted twice with EtOAc
8. washwashed with brine
9. dry with materialdried over Na2SO4
10. customthe solvent was removed
11. customThe residue was triturated with diisopropyl ether
12. customThe precipitate formed
13. filtrationwas filtered off
14. customto give a beige solid (tR 4.08 min (conditions 1)
15. custom16.40 min (conditions 2), MH+=330, 1H-NMR in DMSO-d6: 8.19 (d, 1H); 7.92 (s, 1H); 7.80 (s, 1H); 7.55 (d, 1H); 7.42 (d, 1H); 7.28 (d, 1H); 4.84 (m, 1H); 3.96 (s, 3H); 1.71 (d, 3H)