反应详情

温度

50 °C

Dissolve in 48 ml of toluene 12.0 g (0.03 mol) of trifluoroethanol 2,5-bis-trifluoroethoxybenzoate. Add 3.94 g (0.0345 mol) of 2-aminomethylpiperidine and heat the solution to a temperature of 80°±5° C. for 8 hours. Cool to 50° C. and add 36 ml of water. Carry out the separation at a temperature of 45°±5° C. Concentrate the organic phase under vacuum at a temperature of 35°±5° C. so as to eliminate as much toluene as possible. A semi-solid residue is obtained which is dissolved in 20 ml of methanol and concentrated again to a residue under vacuum. Methanol (40 ml) is then added and heated with refluxing until a yellow solution is obtained. Then cool until the crude base crystallizes, the precipitation is completed by adding 40 ml of water.

1. temperatureheat the solution to a temperature of 80°±5° C. for 8 hours
2. customCarry out the separation at a temperature of 45°±5° C
3. concentrationConcentrate the organic phase under vacuum at a temperature of 35°±5° C. so as
4. customA semi-solid residue is obtained which
5. concentrationconcentrated again to a residue under vacuum
6. additionMethanol (40 ml) is then added
7. temperatureheated
8. temperaturewith refluxing until a yellow solution
9. customis obtained
10. customcrystallizes
11. customthe precipitation
12. additionby adding 40 ml of water