反应详情

温度

-78 °C

n-Butyl lithium (2.5M, 1.1 mL, 2.77 mmol) was added dropwise to a solution of 2-tributylstannanyl-pyrimidine (1 g, 2.71 mmol) in THF (5 mL), under nitrogen at −78° C. 3-Oxo-8-aza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester (0.25 g, 1.13 mmol) in THF (2 mL) was added and the reaction mixture stirred at −78° C. for 3 hours. A solution of saturated aqueous ammonium chloride was added and the mixture extracted into ethyl acetate, dried over magnesium sulphate, filtered and the solvent removed by evaporation under vacuum. The residue was purified by flash chromatography on silica eluting with 5-30% ethyl acetate/cyclohexane. The fractions containing the desired product were concentrated under vacuum to give the title compound (0.14 g). LCMS m/z 306.2 [M+H]+. R.T.=3.44 min (Analytical Method 3).

1. extractionthe mixture extracted into ethyl acetate
2. dry with materialdried over magnesium sulphate
3. filtrationfiltered
4. customthe solvent removed by evaporation under vacuum
5. customThe residue was purified by flash chromatography on silica eluting with 5-30% ethyl acetate/cyclohexane
6. additionThe fractions containing the desired product
7. concentrationwere concentrated under vacuum