P(hpma)-nitrogen mustard polymer with antitumor activity and its preparation method and application
A high-molecular polymer and anti-tumor activity technology, applied in the field of high-molecular chemistry, can solve the problems of high toxicity and side effects, and achieve the effects of reducing toxicity, promoting inhibition, and reducing damage
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Embodiment 1
[0029] A kind of preparation method of the P(HPMA)-nitrogen mustard polymer with antitumor activity, specifically comprises the steps:
[0030] Step (1) N, the synthesis of N-bis-(2-chloroethyl)-4-phenylmethylacrylamide: the step N,N-bis-(2-chloroethyl)-1,4-benzene The hydrochloride (2.7g, 0.01mol) of the amine was first separated and purified with 30% cold NaOH (15ml) solution, then extracted with chloroform (15ml×3), and transferred to the extracted organic solution with pipette Add methacryloyl chloride (0.9678ml, 0.01mol) into the gun, then add triethylamine (1.3899ml, 0.01mol) in trichloromethane solution (5.0ml) dropwise under stirring at 0°C, and control the rate of dropping for 1h The dropwise addition was completed. After the dropwise addition was completed, the ice-water bath was removed, and the reaction was stirred at room temperature for 24 hours. After the reaction was complete, it was washed with distilled water three times (30mL×3), dried overnight with anhydro...
Embodiment 2
[0034] A kind of preparation method of the P(HPMA)-nitrogen mustard polymer with antitumor activity, specifically comprises the steps:
[0035]Step (1) Synthesis of N,N-bis-(2-chloroethyl)-4-benzyl acrylamide: same as Example 1.
[0036] Step (2) Preparation of P(HPMA)-nitrogen mustard polymer with antitumor activity: N, N-bis-(2-chloroethyl)-4-phenylmethylacrylamide (0.0333g) and N-(2-hydroxypropyl) methacrylamide (0.14g) was dissolved with solvent dimethyl sulfoxide (0.3mL), and the initiator azobisisobutyronitrile (0.009g) was added, under nitrogen protection at 65 React at ℃ for 24 hours to polymerize, precipitate with a mixed solution of acetone and ether, and finally centrifuge with an ultrafiltration concentration centrifuge tube with a molecular weight of 3000 to obtain the target polymer.
[0037] Mn=2.1×10 4 , Mw / Mn=1.98. 1 H-NMR (400MHz, d 6 -DMSO, δ, ppm): 3.68(-CH(OH)-ofHPMA,-(CH 2 ) 2 N-),1.33-1.80(-CH 2 -of HPMA), 7.45 (CH of benzene), 7.66 (CH of benzene...
Embodiment 3
[0039] A kind of preparation method of the P(HPMA)-nitrogen mustard polymer with antitumor activity, specifically comprises the steps:
[0040] Step (1) Synthesis of N,N-bis-(2-chloroethyl)-4-benzyl acrylamide: same as Example 1.
[0041] Step (2) Preparation of P(HPMA)-nitrogen mustard polymer with antitumor activity: N, N-bis-(2-chloroethyl)-4-phenylmethylacrylamide (0.0666g) and N-(2-hydroxypropyl) methacrylamide (0.14g) was dissolved with solvent dimethyl sulfoxide (0.3mL), and the initiator azobisisobutyronitrile (0.012g) was added, under nitrogen protection at 65 React at ℃ for 24 hours to polymerize, precipitate with a mixed solution of acetone and ether, and finally centrifuge with an ultrafiltration concentration centrifuge tube with a molecular weight of 3000 to obtain the target polymer.
[0042] Mn=2.6×10 4 , Mw / Mn=2.08. 1 H-NMR (400MHz, d 6 -DMSO, δ, ppm): 3.68(-CH(OH)-ofHPMA,-(CH 2 ) 2 N-),1.33-1.80(-CH 2 -of HPMA), 7.45 (CH of benzene), 7.66 (CH of benzen...
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