Polysaccharide derivative, preparation method thereof and application as chiral stationary phase
A technology of polysaccharide derivatives and chiral stationary phase, which is applied in the field of chiral separation of liquid chromatography, and can solve problems such as difficult chiral resolution materials and poor chiral resolution ability
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Embodiment 1
[0071] Weigh about 0.6g of microcrystalline cellulose and 11.4g of ionic liquid 1-allyl-3-methylimidazolium chloride (AmimCl), put them into a round-bottom flask, heat to 80°C in an oil bath, seal and stir vigorously for 2h . A clear and transparent cellulose solution was obtained, and the concentration of the cellulose solution was 5% (mass fraction). At the same time, 4-tert-butylbenzoyl chloride (about 3.64 g) was added to the solution, so that the molar ratio of 4-tert-butylbenzoyl chloride to cellulose glucose unit was 5:1, and the reaction was performed for 1 h. After the reaction, the crude product was precipitated and washed with methanol, then put into a vacuum drying oven, and baked at 60°C for 24 hours; at the same time, the methanol in the washing liquid was removed by rotary evaporation to realize the recovery of the ionic liquid. 1.8 g of cellulose 4-tert-butylbenzoate with a degree of substitution of 2.58 are obtained. Weigh 1.0 g of cellulose 4-tert-butyl ben...
Embodiment 2
[0073] Weigh about 0.6g of cellulose with a DP of 100, and 11.4g of ionic liquid 1-butyl-3-methylimidazolium chloride (BmimCl), put them into a round bottom flask, heat to 80°C in an oil bath, seal and stir vigorously 2h. A clear and transparent cellulose solution was obtained, and the concentration of the cellulose solution was 5% (mass fraction). At the same time, adamantanecarbonyl chloride (about 4.42 g) was added to the solution so that the molar ratio of adamantanecarbonyl chloride to cellulose glucose unit was 6:1, and the reaction was performed for 1 h. After the reaction, the crude product was precipitated and washed with methanol, then put into a vacuum drying oven, and baked at 60°C for 24 hours; at the same time, the methanol in the washing liquid was removed by rotary evaporation to realize the recovery of the ionic liquid. 2.0 g of cellulose adamantane carboxylate with a degree of substitution of 2.40 was obtained.
[0074] Weigh 1.0 g of cellulose adamantane c...
Embodiment 3
[0076] Weigh about 0.6g of amylose with a DP of 300, and 59.4g of N,N-dimethylacetamide (DMAc), put them into a round bottom flask, heat to 80°C in an oil bath, seal and stir vigorously for 2 hours. A clear and transparent amylose solution was obtained, and the concentration of the amylose solution was 1% (mass fraction). At the same time, α-naphthoyl chloride (about 4.24 g) was added to the solution, so that the molar ratio of α-naphthoyl chloride to amylose glucose unit was 6:1, and the reaction was performed for 2 hours. After the reaction, the crude product was precipitated and washed with methanol, then put into a vacuum drying oven, and baked at 60°C for 24 hours; at the same time, the methanol in the washing liquid was removed by rotary evaporation to realize the recovery of the ionic liquid. 1.5 g of amylose naphthoate with a degree of substitution of 2.68 were obtained.
[0077] Weigh 1.0g of amylose naphthoate with a degree of substitution of 2.68, dissolve it in 20...
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