反应详情

A mixture of {{5-[3,6-dihydro-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazol-3-yl}oxy}acetonitrile (2.63 g, 7.15 mmol) and potassium carbonate (1.97 g, 14.3 mmol) in N,N-dimethylformamide is stirred for 30 minutes, treated with iodomethane (2.03 g, 14.3 mmol), stirred overnight at room temperature, and poured into an ice-water mixture. The resultant aqueous mixture is filtered to obtain a solid. The solid is dissolved in ethyl acetate and the resultant solution is washed sequentially with water and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain a brown solid. Column chromatography of the solid using silica gel and methylene chloride affords a yellow solid. The yellow solid is recrystallized from a methylene chloride/hexanes solution to give the title product as an off-white solid, mp 265-266° C.

1. stirringstirred overnight at room temperature
2. filtrationThe resultant aqueous mixture is filtered
3. customto obtain a solid
4. washthe resultant solution is washed sequentially with water and brine
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated in vacuo
7. customto obtain a brown solid
8. customaffords a yellow solid
9. customThe yellow solid is recrystallized from a methylene chloride/hexanes solution