反应详情

To a stirred solution of 5-bromo-2,4-dichloropyrimidine (500 mg, 2.19 mmol) in MeOH (5 mL) was added a 30% solution of sodium methoxide (0.40 mL, 2.26 mmol). The reaction mixture was stirred at RT for 2 h then concentrated. The residue was dissolved in water (5 mL) and extracted with EA (3×5 mL). The combined organic layer was washed with brine, dried over MgSO4 and concentrated to afford 432 mg (88%) of 5-bromo-2-chloro-4-methoxypyrimidine as white solid. LCMS-ESI (m/z) calculated for C5H4BrClN2O: 223.4. found 224.2 [M+H]+, tR=7.66 min. (Method 2).

1. concentrationthen concentrated
2. dissolutionThe residue was dissolved in water (5 mL)
3. extractionextracted with EA (3×5 mL)
4. washThe combined organic layer was washed with brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated