反应详情

To a solution of 6-bromo-1,4-dihydro-pyrido[2,3-d][1,3]oxazin-2-one (Stage 170.1.3, 0.707 mmol) in DMF (1.4 ml) was added 55% sodium hydride in oil (0.778 mmol). The RM was stirred for 5 min at rt then was added iodomethane (0.778 mmol) and the RM was stirred for 30 min at rt. The RM was diluted with EtOAc, washed with saturated NaHCO3, with brine (3×), dried over Na2SO4, filtered and evaporated. The residue was absorbed on silica gel and separated by flash chromatography (heptane/EtOAc 0% to 70%). The fractions containing product were evaporated together to give the title compound as a yellow solid. (HPLC: tR 2.64 min (Method A).

1. stirringthe RM was stirred for 30 min at rt
2. washwashed with saturated NaHCO3, with brine (3×)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. customevaporated
6. customThe residue was absorbed on silica gel
7. customseparated by flash chromatography (heptane/EtOAc 0% to 70%)
8. additionThe fractions containing product
9. customwere evaporated together