反应详情

2,6Lutidine (18.26 mL) was added to a stirred suspension of (4R,5S)-1,5-dimethyl-4-phenylimidazolidin-2-one (27.33 g) in anhydrous tetrahydrofuran (300 mL) at 0° C. under nitrogen. Bromoacetyl bromide (11.95 mL) was added over 5 minutes and the mixture was stirred for a further 15 minutes. Saturated aqueous sodium bicarbonate solution (300 mL) was added followed by 4-(3,4-dichlorophenoxy)-1-(4-piperidinylmethyl)piperidine (44.86 g) and the mixture was stirred for 24 hours at ambient temperature. Water (300 mL) was added and the mixture was extracted with tert-butyl methyl ether (300 mL). The organic extracts were dried over anhydrous magnesium sulfate, filtered and evaporated under reduced pressure. The residue was suspended in tert-butyl methyl ether (300 mL) and stirred for 3 days. The resulting solid was filtered, washed with tert-butyl methyl ether (3×50 mL) and dried in under reduced pressure to give the title compound (45.65 g) as a solid.

1. stirringthe mixture was stirred for 24 hours at ambient temperature
2. extractionthe mixture was extracted with tert-butyl methyl ether (300 mL)
3. dry with materialThe organic extracts were dried over anhydrous magnesium sulfate
4. filtrationfiltered
5. customevaporated under reduced pressure
6. stirringstirred for 3 days
7. filtrationThe resulting solid was filtered
8. washwashed with tert-butyl methyl ether (3×50 mL)
9. customdried in under reduced pressure