反应详情

温度

0 °C

To a solution of 0.70 g. of 1-methyl-2-nitro-5-imidazolecarboxaldehyde in 180 ml. of diethyl ether, a solution of 0.43 g. of diazomethane in 86 ml. of diethyl ether is added under cooling at about 0° C. After standing at room temperature for 7 days, the reaction mixture is filtered and then evaporated to dryness. The residue (0.60 g.), dissolved in 6 ml. of chloroform, is chromatographed on 6 plates of silica gel, eluting with a 9:1 (v/v) chloroform:methanol mixture, and TLC spots are visualized under U.V. light. The silica gel, which corresponds to an Rf value from 0.64 up to 0.76 is collected and extracted with methanol. From this solution, after filtration and concentration, 0.065 g. of 5-acetyl-1-methyl-2-nitroimidazole is obtained, m.p. 81°-83° C.

1. filtrationthe reaction mixture is filtered
2. customevaporated to dryness
3. dissolutionThe residue (0.60 g.), dissolved in 6 ml
4. customof chloroform, is chromatographed on 6 plates of silica gel
5. washeluting with a 9:1 (v/v) chloroform
6. customis collected
7. extractionextracted with methanol
8. filtrationFrom this solution, after filtration and concentration, 0.065 g