反应详情

温度

52.5 °C

Methyl 4-hydroxy-benzoate (52.0 g, 340 mmols) is suspended in methanesulfonic acid (90 ml) in a round-bottom flask under inert atmosphere, and the mixture is heated to a temperature of 50-55° C. 3-Diisopropylamino-1-phenyl-propan-1-ol (20.0 g, 85.0 mmols) is slowly added thereto in about 2 hours and the hot mixture is reacted for 5-6 hours. The mixture is cooled to room temperature and slowly poured into ice/water (200 g) under strong stirring. The product is extracted with dichloromethane (200 ml) and the organic phase is washed with a 10% sodium hydroxide solution (2×100 ml), then with an ammonium chloride aqueous solution to neutral pH. 28.9 g of product are obtained in 92% yield.

1. customthe hot mixture is reacted for 5-6 hours
2. temperatureThe mixture is cooled to room temperature
3. extractionThe product is extracted with dichloromethane (200 ml)
4. washthe organic phase is washed with a 10% sodium hydroxide solution (2×100 ml)