Preparation method for beta-cyclodextrin chiral stationary phase
A chiral stationary phase, cyclodextrin technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of difficult purification of the reaction, tailing of high performance liquid chromatography peaks, shortened column life, etc. Elution, Ease of Derivatization, Ease of Operation
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Embodiment 1
[0040] Add 7.5g of activated silica gel and 70mL of anhydrous toluene into a 100mL three-necked flask, heat and reflux with a water separator to remove water for 0.5h, then add 4.2mL of 3-aminopropyltriethoxysilane dropwise, and at 100°C The reaction was stirred for 4h. After cooling to room temperature and washing with anhydrous toluene for 5 times, 2.3 mL of trimethylchlorosilane was added dropwise, and the reaction was stirred at 50° C. for 4 h. Cool to room temperature, wash 5 times with anhydrous toluene, take samples and make elemental analysis. Calculate and weigh 3.0g 4,4'-diphenylmethane diisocyanate and add it to the reaction system, 2 , stirred and reacted at 80°C for 6h, cooled to room temperature, and washed 5 times with anhydrous toluene. Calculate and weigh 5.5g β-CD and add it to the reaction system, feed N 2 , Stir the reaction at 80°C for 8h. After cooling to room temperature, it was washed twice with anhydrous toluene, twice with acetone, and three times...
Embodiment 2
[0042] Add 5g of activated silica gel and 70mL of anhydrous toluene into a 100mL three-necked flask, heat and reflux with a water separator and stir to remove water for 0.5h, then add 3.4mL of 3-aminopropyltriethoxysilane dropwise, and stir at 100°C Reaction 4h. After cooling to room temperature and washing with anhydrous toluene for 5 times, 1.8 mL of trimethylchlorosilane was added dropwise, and the reaction was stirred at 50° C. for 4 h. Cool to room temperature, wash 5 times with anhydrous toluene, take samples and make elemental analysis. Calculate and weigh 1.1g 4,4'-diphenylmethane diisocyanate and join in the reaction system, pass into N 2 , stirred and reacted at 80°C for 6h, cooled to room temperature, and washed 5 times with anhydrous toluene. Calculate and weigh 3.9g β-CD and add it to the reaction system, feed N 2 , Stir the reaction at 80°C for 8h. After cooling to room temperature, it was washed twice with anhydrous toluene, twice with acetone, and three tim...
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