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, H NMR spectra were recorded either on Bruker Avance 300 MHz
Avance III HD 400 MHz or NEO 500 MHz at 298 K. 2D NMR (COSY, NOESY, HSQC and HMBC) spectra were recorded on Bruker ,
, Deuterated chloroform (CDCl3) was used as the solvent. NMR chemical shifts were recorded in parts per million referenced to the residual solvent proton
, GC was used to characterize the ratios of diastereomers in the starting vinyl cyclohexeneoxide and the final CHU monomer. The GC spectra were recorded on a GC-2010 Plus (SHIMADZU) instrument
, Size Exclusion Chromatography (SEC) The number-average molecular weights (Mn) and molecular weight distributions of polymers (polydispersity index, PDI) were evaluated by size exclusion chromatography (SEC), using Agilent 1260, Infinity Series GPC
, Monodisperse poly(styrene) polymers were used as calibration standards
Matrix-assisted laser desorption ionization-time of flight mass spectrometry ,
-MS characterization of polymers was performed on UltrafleXtreme mass spectrometer (Bruker Daltonics, Bremen) using trans-2-[3-(4-tert-Butylphenyl)-Chapter V, Materials and methods ,
, 04 mol) was dissolved in 100 mL toluene and triethylamine (TEA, 5.06 g, 0.05 mol) was added dropwise in the ice-water bath. Then ethyl chloroformate (5.43 g, 0.05 mol) was added dropwise in the ice-water bath. The mixture was stirred at room temperature for 3 h. After stopping the reaction, toluene was removed by rotary evaporation and 120 mL water was added. 1:1 as eluent
, 13 C{ 1 H} NMR (CDCl3): ? 157, vol.1
1-hydroxy-2-carbamate-cyclohexane (3, 3.00 g, 16 mmol) was dissolved in 75 mL tetrahydrofuran (THF) and sodium hydride (60 % dispersion in mineral oil, vol.1, p.28 ,
, After stopping the reaction, THF was removed by rotary evaporation and 120 mL water was added. Then the aqueous solution was extracted by EA (3 × 30 mL). The crude product was chromatographed on a silica gel using DCM and EA with a volume ratio of 4:1 as eluent, and the pure product was cyclic urethane 4 (1.88 g, yield: 83%). 1 H NMR (CDCl3): ? 5, vol.15
, Co-first author
Transition from smectic nanofibers to smectic vesicles in the self-assemblies of PEG-b-liquid crystal polycarbonates, Polym. Chem, vol.8, pp.4776-4780, 2017. ,
Polymerization of Cyclic Carbamates: A Practical Route to Aliphatic Polyurethanes ,
URL : https://hal.archives-ouvertes.fr/hal-02357495
Synthesis and self-assembly of polyurethane-based amphiphilic linear diblock copolymers ,
Synthesis and self-assembly of polyurethane-based amphiphilic graft copolymers ,