反应详情

To a solution of sodium (1.63 g, 0.071 mol) in methanol (60 mL) is added dropwise 3-hydroxy-2,4,6-trimethylbenzaldehyde (11.90 g, 0.073 mol) in anhydrous toluene (300 mL). The mixture is heated under reflux and then the methanol is distilled off (volume of azeotropic mixture collected 80-90 mL). After returning to 80-90° C., (2-chloroethyl)imidazolidin-2-one (10.45 g, 0.070 mol) is added all at once to the reaction medium. After heating for 7 hours under reflux, the solvents are evaporated under reduced pressure (Tbath 50° C., 25 mbar). Dichloromethane (150 mL) and water (30 mL) are added to the mixture obtained. The organic phase is then washed twice with water (20 mL). After drying over Na2SO4, the dichloromethane is evaporated under reduced pressure (Tbath 35° C., 33 mbar). Petroleum ether (3 times 50 mL) and water (50 mL) are added to the mixture obtained (24 g) and the precipitate obtained is filtered and washed on the filter with water (15 mL) and petroleum ether (twice 15 mL).

1. temperatureThe mixture is heated
2. temperatureunder reflux
3. distillationthe methanol is distilled off
4. custom(volume of azeotropic mixture collected 80-90 mL)
5. customAfter returning to 80-90° C.
6. temperatureAfter heating for 7 hours
7. temperatureunder reflux
8. customthe solvents are evaporated under reduced pressure (Tbath 50° C., 25 mbar)
9. additionDichloromethane (150 mL) and water (30 mL) are added to the mixture
10. customobtained
11. washThe organic phase is then washed twice with water (20 mL)
12. dry with materialAfter drying over Na2SO4
13. customthe dichloromethane is evaporated under reduced pressure (Tbath 35° C., 33 mbar)
14. additionPetroleum ether (3 times 50 mL) and water (50 mL) are added to the mixture
15. customobtained (24 g)
16. customthe precipitate obtained
17. filtrationis filtered
18. washwashed on the
19. filtrationfilter with water (15 mL) and petroleum ether (twice 15 mL)