反应详情

温度

-78 °C

To a solution of (S)—N-((5-bromo-2-(methylthio)pyrimidin-4-yl)methylene)-2-methylpropane-2-sulfinamide (11C, 2.97 g. 8.8 mmol) in THF (18 mL) cooled to −78° C. was drop wise added 3,5-difluorobenzylmagnesium bromide (53 mL, 0.25 M in Ether, 13.3 mmol). After stirring at −78° C. for 10 min, NH4Cl (sat. aq.) (10 ml) was added to the reaction and warmed up to ambient temperature. Extracted with EtOAc and the organic layer was dried with Na2SO4(s). The solvent was removed and the residue was purified by flash column to yield the title compound (11E) and (S)—N—((S)-1-(5-bromo-2-(methylthio)pyrimidin-4-yl)-2-(3,5-difluorophenyl)ethyl)-2-methylpropane-2-sulfinamide (11D). MS (m/z) 465.87 [M+H]+

1. temperaturewarmed up to ambient temperature
2. extractionExtracted with EtOAc
3. dry with materialthe organic layer was dried with Na2SO4(s)
4. customThe solvent was removed
5. customthe residue was purified by flash column