反应详情

温度

165 °C

2-Chloro-6-trifluoromethyl-benzene-1,4-diamine (2.9 g), bis-(2-chloroethyl)ether (1.7 mL) and sodium iodide (516 mg) were mixed in acetonitrile (45 mL) and heated to 165° C. for 1 hour in a sealed microwave process vessel. The crude mixture was concentrated in vacuo, redissolved in ethyl acetate (100 mL) and washed with water (2×100 mL) and brine (1×100 mL). The organic phase was dried over magnesium sulfate and concentrated in vacuo. The crude product was purified by flash chromatography to furnish 940 mg (24%) of the title compound as a black oil. 1H NMR (500 MHz, CDCl3): 3.02 (m, 4H), 3.84 (m, 4H), 4.30 (b, 2H), 6.97 (d, 1H), 7.06 (d, 1H).

1. concentrationThe crude mixture was concentrated in vacuo
2. dissolutionredissolved in ethyl acetate (100 mL)
3. washwashed with water (2×100 mL) and brine (1×100 mL)
4. dry with materialThe organic phase was dried over magnesium sulfate
5. concentrationconcentrated in vacuo
6. customThe crude product was purified by flash chromatography