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list of experiments
Solubility book (3rd Edn)
Hai Truong and Khalid Mirza
To study the effect of imminium (of phenanthrene-9-carboxaldehyde+ furfurylamine+phenylacetic acid) on the solubility of the Ugi product UCExp176C in methanol
a) phenanthrene-9-carboxaldehyde+ furfurylamine+phenylacetic acid (0.1M, 0.06M, 0.02M) in both benzene and methanol
: Weigh out fufurylamine (0.21mmol, 20mg) in a 2mL volumetric flask. Add a small volume of methanol to it. Then weigh out phenanthrene-9-carboxaldheyde (0.2mmol, 43mg) and add it to the amine/methanol solution, This is imine/methanol solution. Then weigh out phenylacetic acid (0.2mmol, 28mg)and add it to the imine/methanol solution. Make it up to the mark with methanol. Use this as a stock solution-
- 0.06M Pipette out 600uL of 153A in to a 1mL volumetric flask and make it up to the mark with methanol
- 0.02M Pipette out 200uL of 153A in to a 1mL volumetric flask and make it up to the mark with methanol
15:45 Took out a 2ml volumetric flask to make up
solution. Weighted out 20mg of fufurylamine in 2ml volumetric flask. Then added a small amount of methanol to it.
15:50 Weighed out 43mg of phenanthrene-9-carboxaldehyde, and put it into the flask above. Then add a little methanol to it. This is amine/methanol solution.
16:00 Weighed out 28mg of phenylacetic acid, and added it to the flask. Put more methanol to make it to the mark. This was used as stock solution 153A-0.1M
16:10 Took out two 1ml volumetric flasks. Labeled
To flask B: pipetted out 600uL of 153A and put into flask B. Filled up to the mark with methanol.
To flask C: pipetted out 200uL of 153A and put into flask C. Filled up to the mark with methanol.
16:30 Took out three half dram vials. Labeled Exp153-A, Exp153-B and Exp153-C:
: pipetted out 500uL from stock solution 153A. Put small amount of Ugi 176C into it so that there was still small amount of solid remained in the solution.
: pipetted out 500uL from flask B. Put small amount of Ugi 176C into it so that there was still small amount of solid remained in the solution.
: pipetted out 500uL from flask C. Put small amount of Ugi 176C into it so that there was still small amount of solid remained in the solution.
16:40 Parafilmed all the vials
16:45 Put all vials into Lauda heating/cooling bath. The temperature in the bath was 40C
11:10 Changed the temperature setting of the water-glycol to 25C.
16:10 Removed the vials from the temperature control bath and centrifuged them...S
16:20 Obtained six one dram vials and transferred out approximately 400uL DMSO0d6 in to them and labeled
A, B and C
17:00 After centrifuging the half dram vials B through H, carefully transferred out approximately 200uL supernatant from each into corresponding '2' series vials. The resulting solutions in one dram vials with DMSO-d6 are labeled
ONSCExp153A, ONSCExp153B and ONSCExp152C
21:35 Completed obtaining HNMRs of the samples.
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