反应详情

The compound (6-chloro-imidazo[1,2-b]pyridazin-3-yl)-(4-methoxy-phenyl)-methanone (Stage 3.2, 2.04 g, 7.1 mmol) was suspended in ethanol (20 mL) with sodium borohydride (140 mg, 3.6 mmol) and stirred at rt for 7 h. Then water was added and the precipitate formed was filtered off. The yellow solid obtained was dried and then dissolved in TFA (50 mL). Triethylsilane (2.85 mL, 17.7 mmol) was added to the solution and it was stirred at rt for 30 min. the RM was poured into ice water. It was extracted with EtOAc and washed with aqueous 1 N sodium hydroxide solution then with brine. The organic layer was dried over Na2SO4 and concentrated. The residue was purified by chromatography with DCM and MeOH. The title compound was obtained As a white solid (tR 1.1 min (conditions 2), MH+=274).

1. customthe precipitate formed
2. filtrationwas filtered off
3. customThe yellow solid obtained
4. customwas dried
5. dissolutiondissolved in TFA (50 mL)
6. stirringwas stirred at rt for 30 min. the RM
7. extractionIt was extracted with EtOAc
8. washwashed with aqueous 1 N sodium hydroxide solution
9. dry with materialThe organic layer was dried over Na2SO4
10. concentrationconcentrated
11. customThe residue was purified by chromatography with DCM and MeOH