反应详情

温度

25 °C

A solution of 1H-[1,2,4]triazole-3-carboxylic acid methyl ester (3.0 g, 0.23 mol) in N,N-dimethylformamide (76 mL) at 25° C. was treated with triphenylmethylchloride (7.2 g, 0.23 mol) and triethylamine (6.41 mL, 0.23 mol). The reaction mixture was stirred at 25° C. for 4 days and then diluted with ethyl acetate. The mixture was then washed with a dilute aqueous hydrochloric acid solution. At this time, methanol was added to the organic layer. A precipitate formed and was removed by filtration. The organics were further washed with a saturated aqueous sodium chloride solution, dried over magnesium sulfate, filtered, and concentrated in vacuo. The resulting solid was triturated with diethyl ether. The solid was collected by filtration and washed again with diethyl ether to afford 1-trityl-1H-[1,2,4]triazole-3-carboxylic acid methyl ester as a white solid (2.45 g, 84%) which was used without further purification: LR-FAB for C23H19N3O2 (M+) at m/z=369.

1. washThe mixture was then washed with a dilute aqueous hydrochloric acid solution
2. additionAt this time, methanol was added to the organic layer
3. customA precipitate formed
4. customwas removed by filtration
5. washThe organics were further washed with a saturated aqueous sodium chloride solution
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe resulting solid was triturated with diethyl ether
10. filtrationThe solid was collected by filtration
11. washwashed again with diethyl ether