Overall chiral stationary phase of silica gel capillary and preparation method thereof
A technology of chiral stationary phase and capillary monolithic column, which is applied in chemical instruments and methods, and other chemical processes, and can solve the problems of large consumption, chiral reagents that cannot be reused, and chiral immobilization of rosin-based derivatives. , to achieve the effect of low cost, wide solvent selectivity and easy operation
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[0024] (1) Synthesis of maleopimaric acid:
[0025] Take 30.2g of ground-grade rosin in a large beaker, heat it up to 140°C, slowly add 8.82g of maleic anhydride and 1.92g of p-toluenesulfonic acid under constant stirring, then raise the temperature to 180°C, keep it warm for 3 hours, and Pour out heat, grind after cooling, then recrystallize 3 times with glacial acetic acid, filter, and dry to obtain maleopimaric acid (yield 52%), m.p.228-230°C;
[0026] (2) Preparation of silica gel capillary monolithic column:
[0027] Take a quartz capillary with an inner diameter of 75 μm and an outer diameter of 365 μm, soak it with 1mol / L NaoH solution overnight, rinse with secondary water, hydrochloric acid, secondary water, acetone, and anhydrous ether for 1 hour, and then dry it at 180°C for 3 hours under nitrogen flow , sealed at both ends for subsequent use, 0.22g of polyethylene glycol (Mr=10000), 0.225g of urea were dissolved in 0.01mol / L acetic acid solution, wherein 1mL of tet...
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