反应详情

A mixture of 1-(3-methoxyphenyl)-1-propanone (240 g) in 2-propanol (584 ml) is stirred at ambient temperature. Dimethylamine hydrochloride (238.3 g) is added, followed by paraformaldehyde (109.5 g) and an aqueous HCl solution (26.5 ml, 35% w/w). The reaction mixture is heated to reflux temperature and stirred and refluxed for 5 hours. The reaction mixture is allowed to cool to 20° C., and water (730 ml) and toluene (146 ml) are added. The upper organic layer is discarded and an aqueous NaOH solution (50% w/w, 175.2 ml) is added to the water layer while stirring for 10 minutes and keeping the temperature below 25° C. After 10 minutes the layers are allowed to separate, the upper organic layer is isolated and washed with water (219 ml). The organic layer is isolated and concentrated to obtain 3-(dimethylamino)-1-(3-methoxyphenyl)-2-methyl-1-propanone as on oily residue (294.9 g).

1. temperatureThe reaction mixture is heated
2. temperatureto reflux temperature
3. stirringstirred
4. temperaturerefluxed for 5 hours
5. temperatureto cool to 20° C.
6. stirringwhile stirring for 10 minutes
7. customthe temperature below 25° C
8. customto separate
9. customthe upper organic layer is isolated
10. washwashed with water (219 ml)
11. customThe organic layer is isolated
12. concentrationconcentrated