反应详情

温度

20 °C

Into a 50-mL 3-necked round-bottom flask, was placed a solution of 2-((2,4-dichlorobenzyl)(methyl)amino)-1-(4-bromophenyl)ethanol (1.0 g, 2.57 mmol, 1.00 equiv) in dichloromethane (3 mL). This was followed by the addition of conc.H2SO4 (2 mL) dropwise with stirring at 0-5° C. The resulting solution was stirred for 3 h at 20° C. The reaction was then quenched by the addition of water/ice. The pH value of the solution was adjusted to 9 with sodium hydroxide. The resulting solution was extracted with dichloromethane (2×30 mL) and the organic layers combined and dried over anhydrous sodium sulfate and concentrated under vacuum. This resulted in 0.9 g of the title compound which was used without further purification. MS (ES, m/z): 372 [M+H]+.

1. customInto a 50-mL 3-necked round-bottom flask, was placed
2. additionThis was followed by the addition of conc
3. customThe reaction was then quenched by the addition of water/ice
4. extractionThe resulting solution was extracted with dichloromethane (2×30 mL)
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under vacuum