反应详情

温度

60 °C

To a solution of 2-amino-4-chloro-6-methylpyrimidine (Aldrich, 10 g, 70 mmol) in acetonitrile (100 mL) and MeOH (140 mL) was added N-iodosuccinimide (Aldrich, 24 g, 105 mmol) at room temperature. The reaction mixture was heated to 60° C. for 5 h under a nitrogen atmosphere. After the reaction was complete, by monitoring LC/MS, it was allowed to cool to room temperature. The reaction mixture was put on a rotary evaporator and the solvent was evaporated to the half of its original volume. A precipitate was formed by addition of diethyl ether (200 mL). The precipitate was collected by vacuum filtration to afford (15.7 g, 83% yield) of the 4-chloro-5-iodo-6-methylpyrimidin-2-amine; MS (EI) for C5H5ClIN3 (272.65, M+2): analytical HPLC purity >97%.

1. temperatureto cool to room temperature
2. customThe reaction mixture was put on a rotary evaporator
3. customthe solvent was evaporated to the half of its original volume
4. customA precipitate was formed by addition of diethyl ether (200 mL)
5. filtrationThe precipitate was collected by vacuum filtration