反应详情

温度

90 °C

100.0 g (0.92 mol) of (RS)-(+)-2-chloropropionic acid are added to the solution of 192.0 g (0.75 mol) of 4-(5-trifluoromethyl-2-pyridyloxy)phenol in 900 g (about 1050 ml) of xylene. The temperature of the reaction mixture is elevated to 80° C. and 78.0 g (1.95 mol) of sodium hydroxide dissolved in water are added dropwise under such a reduced pressure (about 36 kPa) that the mixture boils at 90° C. The water formed in the reaction is continuously distilled off while maintaining the boiling temperature at 90° C. After the addition, the reaction mixture is stirred at 90° C. for additional 15 minutes, then the reduced pressure is ceased. After adding 300 ml of water to the mixture and stirring at 85° C. for 10 minutes, it is acidified by adding phosphoric acid and the phases are separated. The xylene layer is dried, treated with activated charcoal and finally evaporated to dryness.

1. customis elevated to 80° C.
2. distillationis continuously distilled off
3. additionAfter the addition
4. additionAfter adding 300 ml of water to the mixture
5. stirringstirring at 85° C. for 10 minutes
6. additionby adding phosphoric acid
7. customthe phases are separated
8. dry with materialThe xylene layer is dried
9. additiontreated with activated charcoal
10. customfinally evaporated to dryness