反应详情

To a stirred solution of 4-amino-6-chloro-2-methylthiopyrimidine (3.5 g) in toluene (45 mL) under a nitrogen atmosphere was added, sequentially, 3-(trifluoromethyl)phenylboronic acid (4.15 g), potassium carbonate (25 mL, 2M) and tetrakis(triphenylphosphine)palladium(0) (1.16 g). The mixture was heated to reflux for ten hours. Ethyl acetate (150 mL) was added and the mixture washed with water (2×100 mL). Organic layer was separated, washed with saturated sodium chloride (100 mL), dried over sodium sulphate and solvent was evaporated under reduced pressure to yield crude product. Purification by flash chromatography yielded product 2-methylsulfanyl-6-(3-trifluoromethyl-phenyl)-pyrimidin-4-ylamine (3.45 g)

1. temperatureThe mixture was heated
2. temperatureto reflux for ten hours
3. washthe mixture washed with water (2×100 mL)
4. customOrganic layer was separated
5. washwashed with saturated sodium chloride (100 mL)
6. dry with materialdried over sodium sulphate and solvent
7. customwas evaporated under reduced pressure
8. customto yield crude product
9. customPurification by flash chromatography