Hi All,
I am synthesizing acrylated polycaprolactone (PCL-A) by reacting polycaprolactone (PCL) monomers (Mw: 50k Da) with acryloyl chloride in the presence of a non nucleophilic base i.e. Triethylamine (TEA). I can confirm the successful acrylation of PCL by the manifestation of 3 distinct proton peaks (attributed to end capped acrylate group) at 5.83, 6.12 and 6.4 ppm along with the native PCL peaks at 1.4, 1,65, 2.32 and 4.08 ppm.
However, I need to determine the %yield of the product acrylated PCL. Can somebody help me with the calculation of %yield (or conversion) and the selection of the right proton peaks for the same purpose. I have attached the NMR spectrum of the product (PCL-A).
I am really thankful for your help!
Through integration of a specific proton in both reactant and product, for example if you use ASD lab program. The relative integration percentage of the product proton to the reactant proton. This should be done for a crude NMR sample.
Use an internal standard (eg. trimethylbenzene, TMS) and integrate one of the 1H peaks of the crude and the product. Calculate the ratios of each peak vs. the internal standard and then the use these ratios to calculate the yield (product/crudeX100).
Thanks Aqeel A. Hussein Andrei Blasko for your suggestions. Andrei Blasko I am using d-chloroform (CDCl3) as solvent and it doesn't have TMS in it so I don't get any peak at 0 ppm. I was wondering whether it would be ok to normalize the crude/ product peak integrals against the solvent peak integral (~7.2 ppm for CDCl3) and then calculate the yield%?
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