反应详情

To an ice-cooled solution of 2.02 g (8.3 mmol) of 5-(4-trifluoromethoxy-phenyl)-pent-4-yn-1-ol and 1.73 ml (12.4 mmol) of Et3N in 100 ml of dichloromethane were added 0.67 ml (8.7 mmol) of methanesulfonyl chloride under stirring within 15 min keeping the temperature at 0-10° C. The reaction mixture was stirred at RT for 1 h 15 min. Water was added and after 5 min, the reaction was then partitioned between ether and water. The water was extracted again with ether (two times), the organic phases were washed with aqueous 10% NaCl, dried (Na2SO4) and concentrated to yield 2.50 g of the title compound as light brown oil.

1. customat 0-10° C
2. stirringThe reaction mixture was stirred at RT for 1 h 15 min
3. customthe reaction was then partitioned between ether and water
4. extractionThe water was extracted again with ether (two times)
5. washthe organic phases were washed with aqueous 10% NaCl
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated