Method of synthesising polysaccharide or its derivative modified by phospho lipid group
A technology of phospholipid group and synthesis method, which is applied in the field of biological materials to achieve the effects of good hydrophilicity and biocompatibility
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Embodiment 1
[0028] In a three-neck flask equipped with a constant pressure dropping funnel and a magnetic stirrer, add a part of 100 mesh chitosan powder (by mole fraction, the same below), 3 parts of TEA and 10 parts of dry tetrahydrofuran. After stirring, the reaction system was cooled to -17°C using an ice-salt bath, and three portions of COP dissolved in a certain amount of dry tetrahydrofuran were slowly added dropwise for 3 hours, and then continued to stir for 2 hours. Control the temperature at -17°C. The temperature was naturally raised to room temperature, and the reaction was stirred for 2.5 hours. The solvent THF was removed by suction filtration to obtain the pale yellow product COP-Chitosan.
[0029] Add dry acetonitrile and COP-Chitosan into a thick-walled single-necked flask with a stopper, stir to stabilize the suspension of the system, and then add 20 parts of a saturated solution of acetonitrile containing dry trimethylamine. Close the plunger, put it in a water bath ...
Embodiment 2
[0031] In a three-neck flask equipped with a constant pressure dropping funnel and a magnetic stirrer, add 1 part of chitin film with a thickness of 20 microns, 1 part of triethylamine and 20 parts of toluene. After stirring, the reaction system was cooled to 0°C using an ice-salt bath, and COP dissolved in a certain amount of dry toluene was slowly added dropwise for 2-5 hours, and then continued to stir for 3 hours. Control the temperature at 0°C. The temperature was naturally raised to room temperature, and the reaction was stirred for another 2 hours. The solvent toluene was removed by suction filtration, and the filter residue was vacuum-dried to obtain the yellow product COP-Chitin.
[0032] Add dry acetonitrile and the product from the previous step into a thick-walled single-necked flask with a stopper, stir until the suspension is stable, and then add 10 parts of a saturated acetonitrile solution containing trimethylamine. Close the plunger, put it into a water bath...
Embodiment 3
[0034] In a three-neck flask equipped with a constant pressure dropping funnel and a magnetic stirrer, add 1 part of dry hydroxyethylcellulose powder, 2 parts of triethylamine and dry dioxane. Stir to keep the system in suspension, use an ice-salt bath to cool the reaction system to -10°C, slowly drop in excess 100% COP dissolved in dry dioxane for 2 hours, and then continue to stir for 2 hours. Control the temperature at -10°C. The temperature was naturally raised to room temperature, and the reaction was stirred for another 2 hours. Filtration and vacuum removal of triethylamine chloride gave a yellow product.
[0035] Add dry acetonitrile and the intermediate product into a thick-walled single-necked flask with a stopper, stir to stabilize the suspension, and pass excess dry trimethylamine into it. Close the plunger and put it in a water bath at 100°C for 5 hours. Open the plunger and heat until the residual trimethylamine is driven into the concentrated sulfuric acid. ...
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