反应详情

Benzyltriethylammonium chloride (0.00267 mol) and iodomethane (0.053 mol) were added to a solution of intermediate (74) (0.0267 mol) in concentrated sodium hydroxide (150 ml) and THF (150 ml). The mixture was stirred at room temperature for 4 hours and poured out into ice water. EtOAc was added. The organic layer was separated, washed with water, dried (MgSO4), filtered and the solvent was evaporated. The residue was crystallized from EtOAc/2-propanone. The precipitate was filtered off and dried, yielding 6 g (45%) of 4-(3-chlorophenyl)-6-(3-iodobenzoyl)-1-methyl-2(1H)-quinolinone, melting point 235° C. (intermediate 75).

1. customThe organic layer was separated
2. washwashed with water
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. customthe solvent was evaporated
6. customThe residue was crystallized from EtOAc/2-propanone
7. filtrationThe precipitate was filtered off
8. customdried