反应详情

温度

120 °C

A mixture of N-(5-bromo-2-[2-(trifluoromethoxy)ethyl]amino]phenyl)-3,3-dimethylbutanamide (step C, 728 mg, 1.83 mmol) and p-toluenesulfonic acid monohydrate (350 mg, 1.83 mmol) in toluene (20 mL) was stirred at 120° C. for 8 h. Then, the mixture was allowed to cool to room temperature overnight to afford crystalline precipitates. The precipitates were collected by filtration, and dissolved in ethyl acetate and saturated sodium hydrogencarbonate aqueous solution. The organic layer was separated, washed with brine, dried over magnesium sulfate and concentrated under reduced pressure to afford the title compound (555 mg, 80%) as an amber solid.

1. temperatureto cool to room temperature overnight
2. customto afford crystalline precipitates
3. filtrationThe precipitates were collected by filtration
4. dissolutiondissolved in ethyl acetate
5. customThe organic layer was separated
6. washwashed with brine
7. dry with materialdried over magnesium sulfate
8. concentrationconcentrated under reduced pressure