反应详情

温度

35 °C

To a solution of 2-trifluoromethoxy-5-(4-methyl-piperazin-1-yl)-phenylamine (5.0 g, 0.018 mol), sodium nitrite (5.1 g, 0.0734 mol) in dimethyl sulfoxide (180 mL) a solution of 57% hydroiodic acid (9.6. mL, 0.0427 mol) in dimethyl sulfoxide were added dropwise at room temperature in 20 minutes. The reaction was stirred for 5 hours at 35° C., then cooled in a ice bath and sodium bicarbonate in small portion was added until basic pH. The aqueous layer was extracted with dichoromethane (3×500 mL), the organic phases washed with 10% solution of sodium bisulphite (2×500 mL) then water (1×300 mL). The organic phase was dried over anhydrous Na2SO4, the solvent evaporated under vacuum to yield the intermediate (2.4 g, 34%) as a orange solid which was used as such in the next step.

1. temperaturecooled in a ice bath
2. extractionThe aqueous layer was extracted with dichoromethane (3×500 mL)
3. washthe organic phases washed with 10% solution of sodium bisulphite (2×500 mL)
4. dry with materialThe organic phase was dried over anhydrous Na2SO4
5. customthe solvent evaporated under vacuum