Preparation method of 1,2,3-triazole compound
A technology of azide compounds and compounds, which is applied in the field of polymer/inorganic catalytic synthesis of 1,2,3-triazole compounds, which can solve the problems of shortened reaction time, long reaction time, and easy agglomeration of nano-copper , to achieve the effects of wide application range, simple catalytic system, improved stability and catalytic activity
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Embodiment 1
[0010] Preparation of brominated pullulan ( Carbohydrate Research 2005, 340, 1403-1406)
[0011] Dissolve 5.0g of pullulan in 160ml of DMF (after dehydration treatment), raise the temperature to 60°C, add 13.00g of lithium bromide after 1 hour and stir vigorously for 1 hour, cool down to room temperature, place in an ice-salt bath to drop below 0°C, A mixed solution of 13.8g NBS and 40ml DMF (treated by distillation under reduced pressure) was added dropwise, stirred for 30 minutes, and the reaction mixture was vigorously stirred at 40°C for 6 hours. The reaction mixture was precipitated with acetone, dissolved with DMF, and precipitated with acetone 4 times to obtain purified bromide Pullulan.
Embodiment 2
[0013] The preparation of pullulan triazole ( doi.org / 10.1016 / j.tetlet.2014.02.108)
[0014] The brominated pullulan polysaccharide prepared in Example 1 is used to prepare pullulan triazole, the steps are as follows: respectively weigh brominated pullulan polysaccharide (12mmol), hydroxypropyne (10mmol), NaN 3 (12mmol), CuSO 4 ·5H 2 O (1mol%) and H 2 O (20 mL) was placed in a 100 mL round-bottomed flask, reacted at room temperature for 3 days, the reaction solution was dialyzed with deionized water for 3 days, and freeze-dried to obtain the purified polymer pullulan triazole.
Embodiment 3
[0016] Preparation of organic azides ( Tetrahedron, 2006, 62(50): 11652; J. Mol. Struct., 2008, 892(1-3): 210)
[0017] Weigh 1.95g (30mmol) NaN 3 Add to a 100mL round bottom flask, add 50mL DMF solution, then add 30mmol chlorinated compound, stir overnight at room temperature, after TLC monitors the reaction is complete, pour the reaction solution into 30mL water, CH 2 Cl 2 3×50mL extraction, combined organic phases, washed 3 times with water, dried over anhydrous sodium sulfate, filtered, spin-dried the solvent, purified by column chromatography, and stored at low temperature for use in subsequent reactions.
[0018] The preparation of other benzyl azide compounds is the same as above.
[0019] Weigh 2.42g (15mmol) of o-trifluoromethylaniline and place it in a 50mL round-bottomed flask, then add 10mL of HCl aqueous solution (v: v = 1:1), stir in an ice-water bath at 0-5°C, and then slowly drop Add NaNO 2 Aqueous solution (1.03g, 15mmol NaNO 2 Dissolved in 6mL ice ...
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