反应详情

Methanesulfonyl chloride (3.37 g) was added dropwise to a mixture of 2-[4-(5-methyl-2-phenyl-4-oxazolylmethoxy)phenyl]ethan-1-ol (7.0 g), triethylamine (2.97 g), and ethyl acetate (300 ml) at 0° C., and the mixture was stirred for 3 hours at room temperature. The reaction mixture was poured into water, which was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous sodium bicarbonate, 1N hydrochloric acid and then with saturated aqueous sodium chloride solution, then dried (MgSO4), and concentrated. The crystals obtained were collected by filtration to yield 2-[4-(5-methyl-2-phenyl-4-oxazolylmethoxy)phenyl]ethyl methanesulfonate (8.44 g, yield: 96%). This was recrystallized from ethyl acetate-hexane. Melting point: 66–67° C.

1. extractionwas extracted with ethyl acetate
2. washThe ethyl acetate layer was washed with saturated aqueous sodium bicarbonate, 1N hydrochloric acid
3. dry with materialwith saturated aqueous sodium chloride solution, then dried (MgSO4)
4. concentrationconcentrated
5. customThe crystals obtained
6. filtrationwere collected by filtration