PdBT was synthesized from triblock PGA-PEG-PGA in several steps (Fig. 2A). PGA-PEG-PGA is available commercially but, in this case, was synthesized at a molar feed ratio of 4:1 glycolide:PEG, as described in detail elsewhere (28, 29). PGA-PEG-PGA was dissolved in THF and stirred on ice, followed by addition of 10 mol eq. of TEA and 10 mol eq. of mesyl chloride. After stirring on ice for 8 hours, the product was vacuum-filtered to eliminate particulate side products, precipitated in diethyl ether, redissolved in DCM, and washed twice with ultrapure H2O.

The product of this reaction was then dissolved in acetone, followed by addition of 4 mol eq. of but-2-yne-1,4-dithiol (30) and 4 mol eq. of TEA, and then stirred at ambient temperature for 8 hours. The crude product was then precipitated in diethyl ether, redissolved in DCM, and washed twice with ultrapure H2O. DCM was removed by rotoevaporation, and the final product was dried overnight by vacuum.

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