反应详情

200 mg of soda talc (Merck Catalog No. 1567) were added to a solution of 200 mg of trans-3,4-dihydro-2,2-dimethyl-4-(1-oxoisoindolin-2-yl)-6-trifluoromethylsulfonyl-2H-1-benzopyran-3-ol (prepared as described in Preparation 13) in 6 ml of dioxane, and the resulting mixture was stirred for 30 minutes whilst heating it on an oil bath kept at 140° C. The reaction mixture was cooled and then freed from insoluble materials by filtration. The solvent was then removed by distillation under reduced pressure. The residue was dissolved in 20 ml of methylene chloride, and the resulting solution was washed with water and with a saturated aqueous solution of sodium chloride, in that order. The solution was dried over anhydrous magnesium sulfate, and then the solvent was removed by distillation under reduced pressure. The oily residue thus obtained was recrystallized from ethyl acetate, to afford 81 mg of the title compound, melting at 110°-115° C.

1. temperaturewhilst heating it on an oil bath
2. customkept at 140° C
3. temperatureThe reaction mixture was cooled
4. filtrationfreed from insoluble materials by filtration
5. customThe solvent was then removed by distillation under reduced pressure
6. dissolutionThe residue was dissolved in 20 ml of methylene chloride
7. washthe resulting solution was washed with water and with a saturated aqueous solution of sodium chloride, in that order
8. dry with materialThe solution was dried over anhydrous magnesium sulfate
9. customthe solvent was removed by distillation under reduced pressure
10. customThe oily residue thus obtained
11. customwas recrystallized from ethyl acetate