反应详情

To a solution of 0.25 gram (0.001 mol) of the 1-methyl-5-phenyl-2[(2-oxopropyl)thio]imidazole, prepared as above described, in 10 mL of methylene chloride was added 0.164 g (0.001 mol) of methyl trifluoromethanesulfonate, and the solution was stirred overnight at room temperature. The solvent was evaporated and the residue was converted to the chloride ion form by dissolving in 20% methanol/water and passing through Dowex-1 (Cl-)ion exchange column. The column was eluted with 20 percent methanol in water and the eluate subjected to reduced pressure to evaporate the solvent and to obtain a residue. The residue was stirred overnight in ethyl acetate, filtered and recrystallized from isopropanol/hexane to obtain purified 1,3-dimethyl 4-phenyl-2[(2-oxopropyl)thio]-1H-imidazolium chloride, m.p. 143°-146° C.

1. customThe solvent was evaporated
2. dissolutionby dissolving in 20% methanol/water
3. washThe column was eluted with 20 percent methanol in water
4. customto evaporate the solvent
5. customto obtain a residue
6. filtrationfiltered
7. customrecrystallized from isopropanol/hexane
8. customto obtain
9. custompurified 1,3-dimethyl 4-phenyl-2[(2-oxopropyl)thio]-1H-imidazolium chloride, m.p. 143°-146° C.