反应详情

A mixture of compound 4 (164 g), sodium cyanate (80 g) and manganese dioxide (500 g) in methanol (5.5 l) was stirred at room temperature. Ethanoic acid (122 g) was added dropwise and the resulting reaction mixture was stirred and refluxed overnight. The reaction mixture was filtered over dicalite, and the filter residue was rinsed with CH3OH/CH2Cl2. The filtrate was evaporated. The residue was partitioned between DCM and aqueous K2CO3 solution. The organic layer was separated, dried (MgSO4), filtered and the solvent was evaporated. The residue was crystallized from ACN. The precipitate was filtered off and dried, yielding 152 g (87%) of methyl 6,11-dihydro-11-[1-[2-[4-(2-quinolinylmethoxy)phenyl]ethyl]-4-piperidinylidene]-5H-imidazo[2,1-b][3]-benzazepine-3-carboxylate (compound 6, mp. 179.3° C.).

1. customthe resulting reaction mixture
2. stirringwas stirred
3. temperaturerefluxed overnight
4. filtrationThe reaction mixture was filtered over dicalite
5. washthe filter residue was rinsed with CH3OH/CH2Cl2
6. customThe filtrate was evaporated
7. customThe residue was partitioned between DCM and aqueous K2CO3 solution
8. customThe organic layer was separated
9. dry with materialdried (MgSO4)
10. filtrationfiltered
11. customthe solvent was evaporated
12. customThe residue was crystallized from ACN
13. filtrationThe precipitate was filtered off
14. customdried