反应详情

To a solution of 2-methoxy-6-methylthionaphthalene (1.0 g, 4.9 mmol), [prepared as described in Step 1], in methylene chloride (50 ml) was added 3-chloroperoxybenzoic acid (3.5 g, 10.3 mmol, 50-60%) portionwise. After 0.5 h, the reaction mixture was cooled in an ice bath, sodium sulfite (0.53 g, 4.2 mmol) was added and the stirring was continued for another 20 minutes. The reaction mixture was then poured in water and the organic layer was separated and dried over sodium sulfate. The solvent was removed in vacuo and the crude product was purified by flash chromatography (gradient elution 30-50% ethyl acetate/hexanes) to give 930 mg of 2-methoxy-6-methylsulfonylnaphthalene (80% yield).

1. temperaturethe reaction mixture was cooled in an ice bath
2. waitthe stirring was continued for another 20 minutes
3. customthe organic layer was separated
4. dry with materialdried over sodium sulfate
5. customThe solvent was removed in vacuo
6. customthe crude product was purified by flash chromatography (gradient elution 30-50% ethyl acetate/hexanes)