Beta-cyclodextrin based star-shaped polymer and preparation method thereof

[0039] 1. Preparation of intermediate β-CD-6-OTs

[0040] Add β-cyclodextrin (5.0g, 4.4mmol), sodium hydroxide (1.8g, 45mmol) and 100mL distilled water into a 250mL round-bottomed flask, and stir until completely dissolved; Sulfonyl chloride (TsCl, 1.68g, 8.8mmol), stirred and reacted for 5h, filtered, the filtrate was adjusted to pH 6-7 with 1.0mol / L hydrochloric acid, and then crystallized in ice water; filtered, the filter cake was washed twice with distilled water, The intermediate β-CD-6-OTs (1.07g, 18.9%) was obtained after drying (vacuum drying). 1 H-NMR (DMSO-d 6 , 400MHz, δ): 7.67(d, J=7.5Hz, 2H), 7.36(s, 2H), 4.77(dd, J=42.5, 15.0Hz, 7H), 4.37(s, 7H), 4.29(d, J = 15.2Hz, 7H), 4.17 (dd, J = 14.4, 8.9Hz, 14H), 3.81-3.00 (m, 34H), 2.38 (s, 3H).

[0041] 2. Initiator β-CD-6-NH 2 preparation of

[0042]Accurately weigh β-CD-6-OTs (0.98g, 0.82mmol) and dissolve in 10mL ethylenediamine, 2 protection, stirring and reacting at 70°C for 10 h; after the reaction, under st...

[0048] 1. Preparation of intermediate β-CD-6-OTs

[0049] Take a 250mL single-necked round bottom flask, first add β-cyclodextrin (10g, 8.8mmol), then inject 100mL of 1mol / L NaOH solution, and ultrasonically shake until completely dissolved. Cool the reaction solution in an ice-water bath for 30 min, add p-toluenesulfonyl chloride (TsCl, 3.80 g, 20.0 mmol) dropwise, and react for 5 h under magnetic stirring conditions; / L of hydrochloric acid to adjust the pH to 6-7, cooling and crystallizing in ice water, washing the filter cake obtained after filtration with ethanol and water successively, and drying to obtain the target β-CD-6-OTs (1.42g, yield 12.5%).

[0050] 2. Initiator β-CD-6-NH 2 preparation of

[0051] Accurately weigh β-CD-6-OTs (1.20g, 1.0mmol) and dissolve in 15mL ethylenediamine, 2 protection, stirring and reacting at 70°C for 10 h; after the reaction, under stirring, the reaction liquid was added dropwise to excess ethanol, and the crude product (white preci...