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2 protocols using deuterated dimethyl sulphoxide dmso d6

1

Synthesis and Characterization of OEGMA-AEMA Copolymers

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Oligo(ethylene glycol) methyl ether methacrylate (OEGMA) (average Mn∼ 300 Da), (2-acetoacetoxy)ethyl methacrylate (AEMA) (95%), 2,2-azobis(2-methylpropionitrile) (AIBN) (≥98%), triethylamine (Et3N) (>99%), 1,4-dioxane (anhydrous, 99.8%), n-hexane (anhydrous, 95%), ethyl acetate (anhydrous, 99.8%), deuterated dimethyl sulphoxide (DMSO-d6) (99.9 atom % D), 4-cyano-4-(thiobenzoylthio)pentanoic acid (≥97%), 4-nitrophenol (≥99%), nitrobenzene (≥99%), 3-(4-nitrophenyl)-1,3-oxazolidin-2-one (95%), chloroform (CHCl3) (≥99%), and deuterated chloroform (CDCl3) (99.8 atom % D) were supplied by Merk (Sigma-Aldrich) (Madrid, Spain). Tetrachloroauric (III) acid trihydrate (99%) was supplied by Thermo Scientific (Eindhoven, The Netherlands). Methanol (MeOH, analytical grade) and tetrahydrofuran (THF, GPC grade) were supplied by Scharlau (Barcelona, Spain). Deionized water was obtained from a Thermo Scientific apparatus (Barnstead TII Pure Water System) (Eindhoven, The Netherlands).
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2

Synthesis of Doxorubicin-Loaded PEG Conjugates

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Methoxypoly (ethylene glycol) (mPEG; Mw 2000 g/mol), succinic anhydride (SAA), chloroform-D (CDCl3, 99.8%) and deuterated dimethyl sulphoxide (DMSO-d6) were purchased from Sigma-Aldrich (Shanghai, China); 1-ethyl-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDC·HCl), methyl 4-aminobenzoate and 1-hydroxy-benzotriazole monohydrate (HOBt), from GL Biochem (Shanghai, China); tetramethylethylenediamine, N,N-diisopropyl ethylamine (DIEA) and 4-dimethylaminopyridine (DMAP), from Aladdin Chemistry (Shanghai, China); 1,3-dicyclohexylcarbodiimide (DCC) and cystamine dihydrochloride, from Asta Tech Biopharm (Chengdu, China); and doxorubicin hydrochloride (DOX·HCl), from Shanghai Yingxuan Chempharm (Shanghai, China). DOX was deprotonated as reported [31 (link)]. All solvents were obtained from Chengdu Kelong Chemical (Chengdu, China) and purified before use. Dulbecco's Modified Eagle's Medium (DMEM), Roswell Park Memorial Institute (RPMI) 1640 medium, fetal bovine serum (FBS), and the cell counting kit-8 (CCK-8) were purchased from Life Technologies (Gibco, USA).
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