反应详情

To an ice-cooled solution of 5-(4-trifluoromethoxy-phenyl)-pent-4-yn-1-ol (2.02 g, 8.3 mmol; example 1 a]) and Et3N (1.73 ml, 12.4 mmol) in dichloromethane (100 ml) was added methanesulfonyl chloride (0.67 ml, 8.7 mmol) 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 partitioned between ether and water. The aqueous layer was extracted again with ether (2×), the organic phases were washed with aqueous 10% NaCl, dried (Na2SO4) and concentrated to yield 2.5 g (7.7 mmol, 93%) of the title compound as light brown oil.

1. customat 0-10° C
2. customthe reaction was partitioned between ether and water
3. extractionThe aqueous layer was extracted again with ether (2×)
4. washthe organic phases were washed with aqueous 10% NaCl
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated