反应详情

温度

100 °C

Cesium carbonate (550 mg), L-proline (65 mg), and 1H-1,2,3-triazole (92 mg) were added to a dimethyl sulfoxide (3 ml) solution containing 2-hydroxy-3-iodo-5-nitropyridine (300 mg), and copper iodide (106 mg) was further added in a nitrogen atmosphere, followed by stirring at 100° C. for 3 hours. The reaction solution was adjusted to room temperature. Water and ethyl acetate were added. The pH was adjusted to pH 7 with 1M hydrochloric acid. Insoluble matter was filtered, followed by extraction with ethyl acetate (×3). The resultant was washed with saturated saline and dried over anhydrous sodium sulfate. Subsequently, the solvent was distilled away under reduced pressure, the obtained residue was purified by silica gel chromatography (chloroform:methanol=1:0 to 10:1), and an orange solid of a mixture (184 mg) of 5-nitro-3-(2H-1,2,3-triazol-2-yl)pyridin-2-ol and 5-nitro-3-(1H-1,2,3-triazol-1-yl)pyridin-2-ol was thus obtained.

1. additionwas further added in a nitrogen atmosphere
2. customwas adjusted to room temperature
3. filtrationInsoluble matter was filtered
4. extractionfollowed by extraction with ethyl acetate (×3)
5. washThe resultant was washed with saturated saline
6. dry with materialdried over anhydrous sodium sulfate
7. distillationSubsequently, the solvent was distilled away under reduced pressure
8. customthe obtained residue was purified by silica gel chromatography (chloroform:methanol=1:0 to 10:1)