反应详情

1,1′-Carbonylbis-1H-imidazole (0.02 mol) was added to a solution of (±)-N-(3-aminopropyl)-N′-[(3,4-dihydro-2H-1-benzopyran-2-yl)methyl]-N′-(phenylmethyl)-1,3-propanediamine (0.02 mol) in THF (100 ml). The reaction solution was stirred for 17 hours at room temperature. The solvent was evaporated. Water was added to the residue and the mixture was extracted with toluene. The organic layer was separated, dried, filtered and the solvent evaporated. The residue was crystallized from ethyl acetate (50 ml). The precipitate was filtered off and dried, yielding 3.3 g (42%) of (±)-1-[3-[[(3,4-dihydro-2H-1-benzopyran-2-yl)methyl](phenylmethyl)amino]propyl]-tetrahydro-2(1H)-pyrimidinone (comp. 13); mp. 94.7° C.

1. customThe solvent was evaporated
2. additionWater was added to the residue
3. extractionthe mixture was extracted with toluene
4. customThe organic layer was separated
5. customdried
6. filtrationfiltered
7. customthe solvent evaporated
8. customThe residue was crystallized from ethyl acetate (50 ml)
9. filtrationThe precipitate was filtered off
10. customdried