反应详情

温度

60 °C

At 60° C. a mixture of 30.8 g (0.270 mol) of 4-methylpiperidin-4-ylamine and 100 ml of methanol is added dropwise to a suspension of 100 g (0.257 mol) of (3) in 690 ml of methanol. The mixture is stirred for 1 hour at 60° C., allowed to cool to 40° C., 280 ml of 2N sodium hydroxide solution are added and the resulting mixture is stirred for 3 hours at 60° C. Then 300 ml of methanol are distilled off and 600 ml of water are added. The mixture is stirred for 5 minutes at ambient temperature, filtered off and the residue is washed with 250 ml of water, 3 times 50 ml of acetone and 100 ml of methyl-tert-butylether and dried at 40° C. in vacuo. Yield: 100.5 g (92.2%), melting point 211.5° C. 400 MHz-1H-NMR (DMSO) (ppm)=8.55 br s, 1H, NH; 8.05 dd, 1H, aniline-H; 7.78 ddd, 1H, aniline-H; 7.47 t, 1H, aniline-H; 6.90 br s, 1H, NH; 4.28 s, 2H, CH2; 3.68 m, 2H, CH2; 3.45 m, 2H, CH2, 3.32 br s, 2H, NH2; 1.37 m, 4H, 2CH2; 1.05 s, 3H, CH3.

1. temperatureto cool to 40° C.
2. stirringthe resulting mixture is stirred for 3 hours at 60° C
3. distillationThen 300 ml of methanol are distilled off
4. addition600 ml of water are added
5. stirringThe mixture is stirred for 5 minutes at ambient temperature
6. filtrationfiltered off
7. washthe residue is washed with 250 ml of water, 3 times 50 ml of acetone and 100 ml of methyl-tert-butylether
8. customdried at 40° C. in vacuo
9. custom4.28 s, 2H, CH2
10. custom1.05 s, 3H, CH3