反应详情

A mixture of 3-(bromomethyl)-2,4-dichloropyridine (2.9 g, 12.3 mmol), 2-sulfanyl-6-(trifluoromethyl)pyrimidin-4-ol (1.2 g, 6.1 mmol), and triethylamine (1.3 mL, 9.3 mmol) in absolute ethanol (25 mL) was stirred at room temperature overnight. The mixture was evaporated to dryness. The residue was dissolved in EtOAc (80 mL). The solution was extracted with water (3×50 mL) and 1 N NaOH (1×50 mL). The organic layer was recovered, dried over MgSO4, filtered, evaporated, and dried in vacuo. The crude product was purified by flash chromatography (0-5% MeOH/DCM), affording the title compound (475 mg, 22% yield); 1H NMR (400 MHz, DMSO-d6): δ 4.75 (s, 2H), 6.72 (s, 1H), 7.69 (d, 1H, J=5.3 Hz), 8.36 (d, 1H, J=5.3 Hz); M+ 357.

1. customThe mixture was evaporated to dryness
2. dissolutionThe residue was dissolved in EtOAc (80 mL)
3. extractionThe solution was extracted with water (3×50 mL) and 1 N NaOH (1×50 mL)
4. customThe organic layer was recovered
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customevaporated
8. customdried in vacuo
9. customThe crude product was purified by flash chromatography (0-5% MeOH/DCM)