反应详情

温度

-20 °C

5-Bromo-2,4-dichloro-pyrimidine (2.41 g, 10.6 mmol) is slowly treated with methylamine (8 M in EtOH, 3.3 mL) in THF (15 mL) at about −20° C. After stirring for 30 minutes at about −20° C., the reaction mixture is partitioned between CHCl3 and saturated NaHCO3. The aqueous layer is extracted with additional CHCl3 twice and the combined organic layer is dried over MgSO4, filtered and concentrated. The crude product is purified by column chromatography (SiO2, EtOAc/Hexane=3/7) to give 1.76 g (75%) of (5-bromo-2-chloro-pyrimidin-4-yl)-methylamine as a white solid.

1. customthe reaction mixture is partitioned between CHCl3 and saturated NaHCO3
2. extractionThe aqueous layer is extracted with additional CHCl3 twice
3. dry with materialthe combined organic layer is dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude product is purified by column chromatography (SiO2, EtOAc/Hexane=3/7)