反应详情

To a suspension of 60% sodium hydride oil (3.4 g) in dimethylformamide (25 ml) was added 4-chlorosalicylic acid (7.33 g) under ice-cooling, and the mixture was stirred for 1 hour at room temperature. After the stirring, iodomethane (25 g) was dropwise added to the mixture and the mixture was reacted for 1 hour at 50° C., which was followed by extraction with ether. The extract was washed with water and dried over magnesium sulfate. After the concentration, the residue was chromatographed on silica gel (hexane-ethyl acetate) to give 6.60 g of a colorless transparent liquid (yield 77.4%).

1. temperaturecooling
2. customthe mixture was reacted for 1 hour at 50° C.
3. extractionwhich was followed by extraction with ether
4. washThe extract was washed with water
5. dry with materialdried over magnesium sulfate
6. concentrationAfter the concentration
7. customthe residue was chromatographed on silica gel (hexane-ethyl acetate)