反应详情

A mixture of compound 7 (3 g) and N,N-dimethyl-4-pyridinamine (1.22 g) in DCM (100 ml) was stirred till complete dissolution. 1-(3-Dimethylaminopropyl)-3-ethyl-carbodiimide hydrochloride (1.8 g) was added portionwise and the mixture was stirred at room temperature for 15 minutes. A solution of benzenemethanol (0.54 g) in DCM was added. The mixture was stirred at room temperature overnight. The solvent was evaporated. The residue was purified over silica gel on a glass filter (eluent: CH2Cl2/CH3OH 97/3 to 95/5). The pure fractions were collected and the solvent was evaporated. The residue was crystallized from ACN. The precipitate was filtered off and dried, yielding 2.06 g (62%) of phenylmethyl 6,11-dihydro-11-[1-[2-[4-(2-quinolinylmethoxy)phenyl]ethyl]-4-piperidinylidene]-5H-imidazo[2,1-b][3]benzazepine-3-carboxylate (compound 9).

1. stirringthe mixture was stirred at room temperature for 15 minutes
2. stirringThe mixture was stirred at room temperature overnight
3. customThe solvent was evaporated
4. customThe residue was purified over silica gel on a glass
5. filtrationfilter (eluent: CH2Cl2/CH3OH 97/3 to 95/5)
6. customThe pure fractions were collected
7. customthe solvent was evaporated
8. customThe residue was crystallized from ACN
9. filtrationThe precipitate was filtered off
10. customdried