Preparation method of amylose type derivative functional inorganic-silicon-based chiral micro-sphere fixed-phase material
An amylose, derivative technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of low yield, reduced separation efficiency, tailing, etc., achieve high yield, wide source, solve tailing and other problems Effect
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specific Embodiment approach 1
[0022] 1. Take 0.2g of microcrystalline amylose and vacuum-dry at high temperature for 4h, then stir and reflux in anhydrous N,N-dimethylacetamide for 12h; add lithium chloride after cooling to room temperature (the mass is the mass of amylose After stirring for 3 hours, heat up again, add anhydrous pyridine, add an appropriate amount of 3,5-dimethylphenyl isocyanate (77mol% of the amylose hydroxyl group) after 2 hours of reflux, continue stirring and reflux for 8 hours, and then add a small amount of 3-(trimethoxysilyl) propyl isocyanate (3.1mol% of amylose hydroxyl group), continued to stir and reflux for 12h and then treated with excess 3,5-dimethylphenylisocyanate (90mol% of amylose hydroxyl group ), continue to stir and reflux for 8 hours, then stop the reaction; cool to room temperature, add methanol to settle, filter and wash, and vacuum-dry at 60°C to constant weight, with a yield of 87%. The introduction ratio of 3,5-dimethylphenyl carbamate to 3-(trimethoxysilyl)prop...
specific Embodiment approach 2
[0026] 1. Take 0.2g of microcrystalline amylose and vacuum-dry at high temperature for 4h, then stir and reflux in anhydrous N,N-dimethylacetamide for 12h; add lithium chloride after cooling to room temperature (the mass is the mass of amylose After stirring for 3 hours, heat up again, add anhydrous pyridine, add an appropriate amount of 3,5-dimethylphenyl isocyanate (77mol% of the amylose hydroxyl group) after 2 hours of reflux, continue stirring and reflux for 8 hours, and then add a small amount of 3-(trimethoxysilyl)propyl isocyanate (6.9mol% of amylose hydroxyl group) was treated with excess 3,5-dimethylphenylisocyanate (90mol% of amylose hydroxyl group) after continuous stirring and reflux for 12h , continue to stir and reflux for 8h to stop the reaction; cool to room temperature, add methanol to settle, filter and wash, vacuum dry at 60°C to constant weight, and the yield is 85%. The introduction ratio of 3,5-dimethylphenyl carbamate to 3-(trimethoxysilyl)propyl carbama...
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