A kind of hyperbranched polyphosphoramidite and preparation method thereof
A technology of polyphosphoramidate and hyperbranched polymers, which is applied in the direction of pharmaceutical formulations and medical preparations of non-active ingredients, etc. It can solve the problems of limiting the application of phospholipid polymers and the inability of phospholipid bonds to be degraded by polymers.
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example 1
[0028] Example 1: 0.1 mol of diisopropanolamine and 0.4 mol of triethylamine were dissolved in 50 mL of dichloromethane and 5 mL of DMF, and 0.15 mol of phenyl dichlorophosphate was added thereto under stirring. Reacted at 30°C for 24h, then warmed to 60°C and reacted at this temperature for 24h. After the reaction, the flask was cooled and washed with 2mol / L hydrochloric acid and saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated to the minimum volume under reduced pressure, precipitated with dichloromethane-anhydrous ether three times, and dried in vacuo at 60°C for 24 hours to obtain a pale yellow viscous target polymer. The molecular weight of the product is 6500.
example 2
[0029] Example 2: 0.1 mol of dipropanolamine and 0.4 mol of triethylamine were dissolved in 50 mL of dichloromethane and 5 mL of DMF, and 0.15 mol of phenyl dichlorophosphate was added thereto under stirring. Reacted at room temperature for 24h, then warmed to 60°C and reacted at this temperature for 24h. After the reaction, the flask was cooled and washed with 2mol / L hydrochloric acid and saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated to the minimum volume under reduced pressure, precipitated with dichloromethane-anhydrous ether three times, and dried in vacuo at 60°C for 24 hours to obtain a pale yellow viscous target polymer. The molecular weight of the product is 9500.
example 3
[0030] Example 3: 0.10 mol of dipropanolamine and 0.40 mol of N,N-dimethylaniline were dissolved in 20 mL of tetrahydrofuran and 50 mL of toluene, and 0.15 mol of methyl dichlorophosphate was added thereto under stirring. Reacted at 30°C for 24h, then warmed to 80°C and reacted at this temperature for 48h. After the reaction was completed, the flask was cooled, and the supernatant liquid was poured out. The residual substance was dissolved in chloroform and precipitated in anhydrous ether. The above solvent-precipitation process was repeated three times, and after filtration, washing, and vacuum drying, a white solid was obtained, which was the target polymer. The molecular weight of the product is 27600.
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