A kind of synthetic method of aryl azide and aryl 1,2,3 triazole spiro compound
A technology for a spiro compound and a synthetic method, applied in the field of medicine, can solve the problems of low yield and the like, and achieve the effects of simple operation and high stability
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Embodiment 1
[0030] Add 0.93 g of aniline (10 mmol) into a three-necked flask equipped with a thermometer and a stirrer, add 10 mL of methanol (7.9 g, 0.247 mol) to dissolve it, adjust the pH to 6 with 10% hydrochloric acid, and slowly Feed into 11mmol methyl nitrite to prevent the speed from being too fast, and the reaction is substantially complete after about one hour. Then add 0.98 g of sodium azide (15 mmol) into the three-necked reaction flask, and control the reaction temperature at 80° C., stop the reaction after 1 hour, and obtain a pure product by column separation. Add the azide compound obtained from the above reaction, 0.1 g of α-methylene-γ-butyrolactone (1 mmol) and 10 mL of ethanol (174 mmol) into a three-necked flask, and control the reaction temperature at 60° C. The reaction stopped after 48 hours. The product needs to pass through an alkaline column, and the pure product can be obtained by column separation.
[0031] The product experimental data that embodiment 1 pre...
Embodiment 2
[0037] Add 0.93 g of aniline (10 mmol) into a three-necked flask equipped with a thermometer and a stirrer, add 10 mL of methanol (7.9 g) to dissolve it, adjust the pH to 5 with 10% hydrochloric acid, and slowly introduce 11 mmol of Methyl nitrite, prevent the speed from being too fast, and the reaction is basically complete after 2 hours of reaction. Then add 0.98 g of sodium azide (15 mmol) into the three-necked flask, and control the reaction temperature at 70° C., stop the reaction after 2 hours, and pass through the column to obtain a pure product. Add the azide compound obtained from the above reaction, 0.1 g of α-methylene-γ-butyrolactone (1 mmol) and 10 mL of ethanol into a three-necked flask, and control the reaction temperature at 70° C. The reaction stopped after 36 hours. Column separation yielded pure product.
Embodiment 3
[0039] Add 1.07 g of p-toluidine (10 mmol) into a three-necked flask equipped with a thermometer and a stirrer, add 10 mL of methanol (7.9 g) to dissolve it, adjust the pH to 8 with 10% hydrochloric acid, and slowly Feed into 11mmol methyl nitrite to prevent the speed from being too fast, and the reaction is substantially complete after about one hour. Then add 0.98 g of sodium azide (15 mmol) into the three-necked flask, and control the reaction temperature at 60° C., stop the reaction after 2.5 hours, and obtain a pure product by column separation. Add the azide compound obtained from the above reaction, 0.1 g of α-methylene-γ-butyrolactone and 10 mL of ethanol into a three-necked flask, and control the reaction temperature at 50°C. The reaction stopped after 72 hours. The product needs to pass through an alkaline column, and the pure product can be obtained by column separation.
[0040] The product experimental data that embodiment 3 prepares is as follows:
[0041] 1b:...
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