反应详情

(S)-2-Chloro-1-(2-hydroxy-2-methyl-3-methanesulfonyloxypropyl)-4-nitroimidazole prepared in Example 17 (3.02 g, 9.51 mmol) was dissolved in methylene chloride (30 ml). DBU (1.7 ml, 11.41 mmol) was added to the solution, and the resulting mixture was stirred at room temperature for 1.5 hours. The reaction mixture was washed with 3N hydrochloric acid (30 ml) and saturated saline solution (20 ml) in this order, dried over magnesium sulfate and then filtered. The filtrate was concentrated and the residue was purified by silica gel column chromatography (methylene chloride/ethyl acetate=20/1) to afford (S)-2-chloro-1-(2-methyloxiran-2-ylmethyl)-4-nitroimidazole (1.89 g, yield 91%) as a light yellow solid.

1. washThe reaction mixture was washed with 3N hydrochloric acid (30 ml) and saturated saline solution (20 ml) in this order
2. dry with materialdried over magnesium sulfate
3. filtrationfiltered
4. concentrationThe filtrate was concentrated
5. customthe residue was purified by silica gel column chromatography (methylene chloride/ethyl acetate=20/1)