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14th November 2016 @ 16:54
11/9/16 Purification:   The 550 mg of MSLR 9-1 was dry loaded onto silica and the product was purified using the biotage using a solvent system of 100% ETOAc. Fractions containing product were checked using TLC. TLC shows that the product was successfully isolated. In 3 fractions, high Rf impurities might be present in low concentration, however it is unclear and this will be addressed if the NMR looks messy. The product was concentrated in vacuo. Yield: 0.145 grams 100% EtOAc solvent system, silica gel plate, UV visualization The numbers at the bottom of the TLC plates are the factions we identified our product to be in.  The curve seen between the factions on the TLC suggests there are diastereomers present in our final product.     11/10/2016 4. Used HNMR to determine if THP and BOC groups were present in the product. The tall peak at approximately 1.5 ppm suggests the presence of a BOC group (the 9H on the quaternary carbon at the end). The presence of peaks between 3-4 pm, as well as others around 1 ppm suggest THP is present .  [data]20357[/data]   Conclusions:   It appears that the protecting groups are present. A deprotection step will be done to see if the final product is successfully synthesized.
Attached Files
purificationCarbonNMR.pdf