反应详情

To N-(5-bromo-2-methoxy-pyridin-3-yl)-acetamide (Stage 62.1.3, 100 mg, 0.408 mmol) DMF (1 ml) was added NaH 55% in oil (19.6 mg, 0.45 mmol). The reaction mixture was stirred for 10 min at rt then was added MeI (0.031 ml, 0.49 mmol). The reaction mixture was stirred for 1 h at rt then quenched with brine and extracted with EtOAc (2×). The organic layers are washed with brine (3×), dried over Na2SO4, filtered and evaporated. The crude product was purified by Prep.HPLC. The fractions containing the product were collected together and basified with NaHCO3, before being concentrated and extracted with EtOAc (3×). The organic layers were dried over Na2SO4, filtered and evaporated to dryness to give the title compound as an off-white solid (HPLC: tR 2.75 min (Method A); M+H=259, 261 MS-ES).

1. stirringThe reaction mixture was stirred for 1 h at rt
2. customthen quenched with brine
3. extractionextracted with EtOAc (2×)
4. washThe organic layers are washed with brine (3×)
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customevaporated
8. customThe crude product was purified by Prep.HPLC
9. additionThe fractions containing the product
10. customwere collected together
11. concentrationbefore being concentrated
12. extractionextracted with EtOAc (3×)
13. dry with materialThe organic layers were dried over Na2SO4
14. filtrationfiltered
15. customevaporated to dryness