反应详情

To a solution of 1.00 g of the compound obtained in Step 179-1 in CHCl3 (10 ml) was added dropwise 3.36 g of chlorosulfonic acid in CHCl3 (10 ml) over 30 minutes under ice cooling. After stirring at room temperature for one hour, the solution was poured into ice water and the resulting mixture was extracted with CHCl3. The organic layer was washed with a saturated aqueous solution of NaHCO3 and with saturated brine and then dried over MgSO4; the drying agent was separated by filtration, and then the solvent was evaporated under reduced pressure. The obtained residue was purified by column chromatography (silicagel 60N; mobile phase: EtOAc/n-hexane=1/10 to 1/5; v/v) to obtain 340 mg of 4-(methylthio)-2-(trifluoromethoxy)benzene sulfonyl chloride (179-2-a) and 212 mg of 2-(methylthio)-4-(trifluoromethoxy)benzene sulfonyl chloride (179-2-b).

1. extractionthe resulting mixture was extracted with CHCl3
2. washThe organic layer was washed with a saturated aqueous solution of NaHCO3 and with saturated brine
3. dry with materialdried over MgSO4
4. customthe drying agent was separated by filtration
5. customthe solvent was evaporated under reduced pressure
6. customThe obtained residue was purified by column chromatography (silicagel 60N; mobile phase: EtOAc/n-hexane=1/10 to 1/5; v/v)