Preparation of bonding- affinity composite type polysaccharides chiral stationary phase
A chiral stationary phase, composite technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of low solubility of chiral substances, weak physical coating binding force, low resolution ability, etc., to avoid The loss of chiral selector, the effect of overcoming the low chiral resolution and expanding the scope of use
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[0014] Example 1
[0015] Take 1 g of cyclodextrin and put it into a reactor containing 30 mL of pyridine, then add 3,5-dichlorophenyl isocyanate equivalent to 1.5 times the amount of cyclodextrin, and react at 80° C. for 24 hours. After cooling, a large amount of methanol was added to precipitate the product, and after filtration and washing, the product was vacuum-dried to constant weight to obtain the polysaccharide derivative (I) whose hydroxyl substitution degree was 50%; under other conditions unchanged, change 3, The amount of 5-dichlorophenyl isocyanate used is 1.87 times that of cyclodextrin, that is, the polysaccharide derivative (II) whose hydroxyl substitution degree is 60% is obtained.
[0016] Take 1 g of polyacrylic acid into a round-bottomed flask, add 10 mL of pyridine, swell for 1 hour, add 1.5 mL of thionyl chloride, react at 50°C for 8 hours, remove the unreacted sulfoxide chloride, and then add 1 g of polysaccharide derivative Compound (I) and 10 mL of ac...
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[0018] Example 2
[0019] Take 1 g of starch and put it into a reactor containing 20 mL of pyridine, then add 3,5-dimethylphenyl isocyanate equivalent to 1.3 times the amount of starch, and react at 100° C. for 24 hours. After cooling, a large amount of ethanol was added to precipitate the product, and after filtration and washing, the product was vacuum-dried to a constant weight to obtain the polysaccharide derivative (I) whose hydroxyl substitution degree was 45%; The amount of 5-dimethylphenyl isocyanate is 3.0 times that of starch, that is, the polysaccharide derivative (II) whose hydroxyl substitution degree is 80% is obtained.
[0020] Take 1 g of carboxymethyl cellulose into a round-bottomed flask, add 10 mL of tetrahydrofuran, swell for 8 hours, add 4 mL of thionyl chloride, react at 50°C for 8 hours, remove the unreacted sulfoxide chloride, and then add 1 g The polysaccharide derivative (I) and 10 mL of tetrahydrofuran were stirred to disperse uniformly, and reacted...
Example Embodiment
[0022] Example 3
[0023] Take 1 g of cellulose and add it to a reactor containing 15 mL of pyridine, then add phenyl isocyanate equivalent to 0.9 times the amount of cellulose, and react at 80° C. for 24 hours. After cooling, a large amount of methanol was added to precipitate the product, and after filtration and washing, the product was vacuum-dried to a constant weight to obtain the polysaccharide derivative (I) whose hydroxyl substitution degree was 39%; When the amount of isocyanate is 5 times that of cellulose, the polysaccharide derivative (II) is obtained with a hydroxyl substitution degree of 95%.
[0024] Take 1 g of carboxylated polystyrene into a round-bottomed flask, add 10 mL of dichloromethane, swell for 12 hours, add 0.75 mL of thionyl chloride, and react at 40°C for 8 hours. 1 g of the polysaccharide derivative (I) and 10 mL of pyridine were sequentially added, stirred to disperse uniformly, and reacted at 80° C. for 12 hours. After cooling, the product is ...
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