Objective

To determine the solubility of UC214F-2 and Boc-glycine, veratraldehyde and piperonal in different solvents by NMR.

Procedure

Saturated solutions of Ugi product 215C, Boc-glycine, piperonal and veratraldehyde were prepared in different solvents in one dram vials, after vortexing excess solute in each for 10min. The solutions were left to equilibrate betweeen 24-48h. The solutions were then centrifuged and the supernatants were decanted in to separate vials. The supernatants (100uL) were dissolved in CDCl3 and a proton NMR was obtained on a 500MHz varian instrument. The concentration of the solute was determined using SAMS.

Results

Saturated solutions
215C; HNMR in CDCl3
Boc-glycine;HNMR in CD3OD
piperonal; HNMR in CD3OD
veratraldehyde; HNMR in CD3OD

Spreadsheet


Conclusion

Solubility of the Ugi product 215C, piperonal, veratraldehyde and Boc-glycine has been determined in different solvents.


Log


2009-03-19

13:00 Made-up saturated solutions of UC215F-2 in methanol, ethanol, THF, acetonitrile, toluene and DMSO. After the last addition of the solute each solution was vortexed for 10min to ensure saturation.
17:00 Made-up saturated solutions of Boc-glycine in methanol, ethanol, THF, acetonitrile, toluene, DMSO, hexane, diethylether, chloroform and dichloromethane. After the last addition of the solute each solution was vortexed for 10min to ensure saturation. Chloroform, dichloromethane and toluene formed gels.
18:00 Left the solutions overnight to equilibrate.

2009-03-20

12:00 Made-up saturated solutions of veratraldehyde in methanol, ethanol, THF, acetonitrile, toluene and DMSO, hexane, diethylether, chloroform and dichloromethane. After the last addition of the solute each solution was vortexed for 10min to ensure saturation.

2009-03-21

10:30 Centrifuged the solutions to make sure the supernatants were completely separated from solute.
11:30 Prepared solutions for NMR analysis by dissolving 100uL of each supernatant in 700uL CDCl3.
19:50 Obtained NMR of all the solutions.