Preparation method of hyperbranched polymers with redox responsiveness
A hyperbranched polymer and responsive technology, applied in the chemical field, can solve problems such as complex and lengthy synthesis processes, and restrictions on the commercial application of ABn-type monomers
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Embodiment 1
[0033] (1) 3,3'-Dipropyne dithiodipropionate (A 2 monomer) synthesis
[0034] 3,3'-dithiodipropionic acid (6.31 g, 30 mmol) and DMAP (0.183 g, 1.5 mmol) were dissolved in 60 ml of anhydrous THF, then EDC (5.75 g, 30 mmol) was dissolved in propargyl alcohol (4.48g, 80mmol), was added dropwise to the mixed solution through a constant pressure dropping funnel under the condition of an ice-water bath. The mixture was stirred at room temperature for 48 h, then the solvent was evaporated in vacuo. The residue was dissolved in ethyl acetate, washed with saturated brine, and washed with anhydrous MgSO 4 The extract was dried (stand overnight), and the magnesium sulfate hydrate was removed by filtration. Select dichloromethane as the eluent, purify through a silica gel column (70-230 mesh silica gel), rotate the fraction collected after passing through the silica gel column, combine the products and concentrate to obtain a colorless liquid (5.17g) (such as figure 1 , figure 2 ). ...
Embodiment 2
[0048] Note: in the present invention dithiodipropionate dipropyne (A 2 monomer), tris(1-chlorobutyrate)ethane and tris(1-azidobutyrate)ethane with azide (B 3 The preparation of the monomer) is consistent with that described in Example 1, and only the hyperbranched polymer preparation method of different terminal groups is introduced in the following examples.
[0049] Dipropyne 3,3'-dithiodipropionate (A 2 monomer) (0.57g; 2mmol) and tris(ethyl-1-azidobutyrate)ethane (B 3 monomer) (0.675g; 1.5mmol) was dissolved in 12ml of anhydrous DMF, under N 2 Add PMDETA (0.116g; 0.67mmol) under the atmosphere, continue to pass N 2 After about 30min, at N 2 Cuprous bromide (0.096g; 0.067mmol) was added under the atmosphere, the reaction solution was light green, and it was sealed and reacted at room temperature for 24h. After the reaction, the reactants were dissolved in DMF, and stirred for a period of time, so that the cuprous ions were completely oxidized to copper ions, and DMF w...
Embodiment 3
[0052]Note: in the present invention dithiodipropionate dipropyne (A 2 monomer) and tris(1-azidobutyrate ethyl)ethane with azide (B 3 The preparation of the monomer) is consistent with that described in Example 1, and only the hyperbranched polymer preparation method of different terminal groups is introduced in the following examples.
[0053] Dipropyne 3,3'-dithiodipropionate (A 2 monomer) (1.14g; 4mmol) and tris(ethyl-1-azidobutyrate)ethane (B 3 monomer) (0.9g; 2mmol) was dissolved in 20ml of anhydrous DMF, under N 2 Add PMDETA (0.116g; 0.67mmol) under the atmosphere, continue to pass N 2 After about 30min, at N 2 Cuprous bromide (0.096g; 0.067mmol) was added under the atmosphere, the reaction solution was light green, and it was sealed and reacted at room temperature for 24h. After the reaction, the reactants were dissolved in DMF, and stirred for a period of time, so that the cuprous ions were completely oxidized to copper ions, and DMF was used as the eluent, and pu...
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