Objective


Test the solubility of Ugi Product 216-4A in THF, methanol, acetonitrile, DMSO, and toluene.

Results


Spreadsheet


Discussion


Conclusion


Log


5-22-2009

Vial Label
Solvent
1
THF
2
Methanol
3
Acetonitrile
4
DMSO
5
Toluene


9:58: One half dram vials was labeled 1. 250uL of THF was pippeted into vial 1. Ugi Product was added to vial 1. The vial was vortexed for 20 seconds. After several trials of adding Ugi Product and vortexing for 20 seconds, the solution appeared to be saturated. The solution appeared cloudy and solid was forming at the bottom. After several minutes (before sonication), solid formed at the bottom and the solution appeared to be clear.

10:02: One half dram vials was labeled 2. 250uL of methanol was pippeted into vial 1. Ugi Product was added to vial 1. The vial was vortexed for 20 seconds. After several trials of adding Ugi Product and vortexing for 20 seconds, the solution appeared to be saturated. The solution appeared cloudy and solid was forming at the bottom. After several minutes (before sonication), solid formed at the bottom and the solution appeared to be clear.

10:06: One half dram vials was labeled 3. 250uL of acetonitrile was pippeted into vial 1. Ugi Product was added to vial 1. The vial was vortexed for 20 seconds. After several trials of adding Ugi Product and vortexing for 20 seconds, the solution appeared to be saturated. The solution appeared cloudy and solid was forming at the bottom. After several minutes (before sonication), solid formed at the bottom and the solution appeared to be clear.

10:09: One half dram vials was labeled 4. 250uL of DMSO was pippeted into vial 1. Ugi Product was added to vial 1. The vial was vortexed for 20 seconds. After several trials of adding Ugi Product and vortexing for 20 seconds, the solution appeared to be saturated. The solution appeared cloudy and solid was forming at the bottom. After several minutes (before sonication), solid formed at the bottom and the solution appeared to be clear.

10:12: One half dram vials was labeled 5. 250uL of toluene was pippeted into vial 1. Ugi Product was added to vial 1. The vial was vortexed for 20 seconds. After several trials of adding Ugi Product and vortexing for 20 seconds, the solution appeared to be saturated. The solution appeared cloudy and solid was forming at the bottom. After several minutes (before sonication), solid formed at the bottom and the solution appeared to be clear.

10:19 Vials 1-4 were placed in a small beaker with some water. Since the beaker was not large enough for all 5 solutions, Vial 2 was placed in a small beaker by itself. These beakers were placed in a sonicator. The bath temperature was 26C. The sonicator was turned on and set to 30 minutes.

10:25: The lids of vials 2 and 4 came off multiple times during sonicator. Water did not appear to spill in these vials.

10:39 All vials were removed from the sonicator. The bath temperature was 41C. Only vial 5 had solid at the bottom.

10:41 More Ugi product was added to vials 1-4. They were vortexed for 20 seconds. After several trials of adding Ugi and vortexing, vials 1-4 appeared to be saturated.

10:56 Vials 1-4 were placed in a small beaker with some water. The beaker was placed in a sonicator. The bath temperature was 37C. The sonicator was turned on and set to 30 minutes.

11:26: The beaker was removed from the sonicator. The bath temperature was 46C. All vials had solid formed at the bottom. Since there were no clean NMR tubes available, parafilm was placed over each vial. All solutions were left on the workbench.

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