反应详情

1-[4-[4-[[2-[(E)-2-[4-(Trifluoromethyl)phenyl]ethenyl]-1,3-oxazol-4-yl]methoxy]phenyl]butyl]-1H-1,2,3-triazole (1.0 g) was dissolved in ethyl acetate (50 ml) and tetrahydrofuran (5 ml). A solution of methanesulfonic acid (205 mg) in tetrahydrofuran (5 ml) was added dropwise. The crystals were precipitated. The mixture was stirred at room temperature for 20 min and under ice-cooling for 50 min. The reaction mixture was concentrated under reduced pressure until the liquid amount became about half. After stirring the mixture under ice-cooling for 30 min, the mixture was filtrated, washed with ethyl acetate/isopropyl ether=1/1 (3 ml) and dried under reduced pressure (40° C.) to give 1-[4-[4-[ [2-[ (E)-2-[4-(trifluoromethyl)-phenyl]ethenyl]-1,3-oxazol-4-yl]methoxy]phenyl]butyl]-1H-1,2,3-triazole methanesulfonate (1.18 g, yield 98%).

1. customThe crystals were precipitated
2. temperaturecooling for 50 min
3. concentrationThe reaction mixture was concentrated under reduced pressure until the liquid amount
4. stirringAfter stirring the mixture under ice-
5. temperaturecooling for 30 min
6. filtrationthe mixture was filtrated
7. washwashed with ethyl acetate/isopropyl ether=1/1 (3 ml)
8. customdried under reduced pressure (40° C.)