反应详情

Under nitrogen atmosphere, 200 mg of trifluoromethanesulfonate 5-oxo-5,6,7,8-tetrahydro-naphthalene-2-ylester was dissolved in 3 ml of dimethylformamide. 54 mg of 60% sodium hydroxide and 1.0 ml of methyl iodide were added and the mixture was stirred at room temperature for 2 hours. Water was added to the reaction solution, extracted with ethyl acetate. Ethyl acetate layer was washed with saturated saline solution, and dried with anhydrous sodium sulfate. The solvents were distilled outunder reduced pressure, and the residues were separated and purified by preparative thin-layer chromatography (ethyl acetate/hexane=1/2) to obtain 42 mg of the above compound as a yellow oily matter.

1. extractionextracted with ethyl acetate
2. washEthyl acetate layer was washed with saturated saline solution
3. dry with materialdried with anhydrous sodium sulfate
4. distillationThe solvents were distilled outunder reduced pressure
5. customthe residues were separated
6. custompurified by preparative thin-layer chromatography (ethyl acetate/hexane=1/2)