反应详情

温度

50 °C

47.2 g (0.413 mol) of 1-methyl-4-aminopiperidine is added dropwise at ambient temperature to a mixture of 123.3 g (0.317 mol) of (3), 740 ml of THF and 61.7 ml (0.445 mol) of triethylamine. The mixture is stirred for 30 min at 50° C. It is left to cool to 40° C., 1480 ml of water are added and the mixture is then stirred for 90 minutes at 10° C. The product that crystallises out is filtered off, washed with 150 ml of water and dried in vacuo at 60° C. The product is dissolved in 1150 ml of ethyl acetate at boiling temperature. It is cooled to 10° C., filtered and the product that crystallises out is dried at 60° C. in vacuo. Yield: 128.9 g (87.2%).

1. waitIt is left
2. temperatureto cool to 40° C.
3. stirringthe mixture is then stirred for 90 minutes at 10° C
4. customThe product that crystallises out
5. filtrationis filtered off
6. washwashed with 150 ml of water
7. customdried in vacuo at 60° C
8. dissolutionThe product is dissolved in 1150 ml of ethyl acetate
9. temperatureIt is cooled to 10° C.
10. filtrationfiltered
11. customthe product that crystallises out
12. customis dried at 60° C. in vacuo