反应详情

温度

25 °C

To a stirred mixture of 1-methyl-3-(pyrrolidin-1-yl)-1H-1,2,4-triazole-5-carbaldehyde (1.57 g, 8.71 mmol, Eq: 1.00) and potassium carbonate (2.41 g, 17.4 mmol, Eq: 2) at 25° C. in methanol (60 ml) under an argon atmosphere was added dropwise a solution of dimethyl 1-diazo-2-oxopropylphosphonate (2.01 g, 1.57 ml, 10.5 mmol, Eq: 1.2) in methanol (12 ml). The mixture was stirred at 25° C. for 3 h. The crude material was applied on silica gel and purified by flash chromatography over a 50 g silica gel column using dichloromethane/methanol 0-10% as eluent affording 5-ethynyl-1-methyl-3-pyrrolidin-1-yl-1H-[1,2,4]triazole (785 mg, 51.1%) as an orange solid. MS: m/z=149.2 (M+H+)

1. custompurified by flash chromatography over a 50 g silica gel column