反应详情

温度

0 °C

To a solution of 2-[3,5-dichloro-4-(4-methoxy-3-nitro-phenoxy)-phenyl]-2H-[1,2,4]-triazin-3,5-dione (1.32 g, 3.1 mmol) in 12 mL of DMF at 0° C. was added sodium hydride (60% dispersion in mineral oil, 0.15 g, 3.7 mmol). After stirring at 0° C. for 5 min, the mixture was stirred at room temperature for 30 min as a clear reddish brown solution. To the solution at room temperature was added SEMCl (0.63 g, 3.74 mmol). After stirring at room temperature for 20 h, the solution was diluted with H2O (30 mL) and extracted with EtOAc (2×50 mL). The combined EtOAc extracts were washed with 1N HCl (100 mL), H2O (3×50 mL), brine (100 mL), dried and concentrated. The residue was dissolved in CH2Cl2followed by addition of ether to give the title compound (0.83 g) of Step A as light brown crystals. NMR (400 Mhz, CD3OD) d 0.02 (m, 9H), 1.01 (m, 2H), 3.75 (m, 2H), 5.45 (s, 2H).

1. stirringthe mixture was stirred at room temperature for 30 min as a clear reddish brown solution
2. stirringAfter stirring at room temperature for 20 h
3. extractionextracted with EtOAc (2×50 mL)
4. washThe combined EtOAc extracts were washed with 1N HCl (100 mL), H2O (3×50 mL), brine (100 mL)
5. customdried
6. concentrationconcentrated
7. dissolutionThe residue was dissolved in CH2Cl2followed by addition of ether