反应详情

A mixture of intermediate (5-a) (21.2 g) in hydrochloric acid (3 N) (150 ml) and 2-propanol (150 ml) was stirred and refluxed overnight. The mixture was poured into ice, basified with NH4OH and extracted with DCM. The organic layer was dried (MgSO4), filtered off and evaporated till dryness. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2 /CH3OH/NH4OH 98/2/0.1). The pure fractions were collected and evaporated, yielding 11.6 g (59%) of (±)-6-[amino-(4-chlorophenyl)methyl]-1-methyl-4-phenyl-2(1H)-quinolinone (interm. 5-b).

1. temperaturerefluxed overnight
2. additionThe mixture was poured into ice
3. extractionextracted with DCM
4. dry with materialThe organic layer was dried (MgSO4)
5. filtrationfiltered off
6. customevaporated till dryness
7. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2 /CH3OH/NH4OH 98/2/0.1)
8. customThe pure fractions were collected
9. customevaporated