[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[CH2:9][CH2:10][CH2:11][OH:12].C(N(CC)CC)C.[CH3:20][S:21](Cl)(=[O:23])=[O:22]>C(Cl)Cl.[Cl-].[Na+].O>[CH3:20][S:21]([O:12][CH2:11][CH2:10][CH2:9][C:3]1[C:2]([Cl:1])=[CH:7][CH:6]=[CH:5][C:4]=1[Cl:8])(=[O:23])=[O:22]To a solution of 3-(2,6-dichlorophenyl)-1-propanol (125 mg, 0.61 mmol) and triethylamine (123 mg, 1.22 mmol) in methylene chloride (3 mL), methanesulfonyl chloride (105 mg, 0.915 mmol) was added under ice cooling, followed by stirring at room temperature for 2 hours. Brine was added to the reaction mixture. The organic layer was allowed to separate, was collected, and was then dried over anhydrous sodium sulfate. Subsequent to concentration under reduced pressure, the residue was purified by chromatography on a silica gel column (hexane/ethyl acetate=10/1) to yield the title compound as a pale yellow syrupy substance (yield: quantitative).
読み込み中…
