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list of experiments
Solubility book (3rd Edn)
To determine the concentration of saturated solutions of the Ugi product
in 17 unique solvents and 3 binary solvent systems
[It looks like all the spectra are in the spreadsheet - just need to set the ranges - you should be able to conclude this experiment now JCB]
11:00 Labeled 20 one dram screw top vials.(1-20).
11:15 Placed a small amount of the Ugi product
in those vials.
11:45 Pipetted out 400uL of the solvents listed in the table below in to corresponding vial. Each vial was vortexed for approximately for 15s each after the addition of solvent.
14:20 Placed the vials in to a bath at 46C.
16:00 Solutions in a few vials had gotten clear, therefore extra solute was added to these vials and placed back in to the hot bath at 46C.
18:00 All vials still contained some amount of solid in them. Temperature of the bath was now programed to 23C.
18:20 Temperature of the bath 23C.
15:30 Removed vials 1, 2, 3, 4, 5, 6, 9, 11, 12, 13, 16, 17, and 18 from bath. Vials not mentioned (8, 10, 14, and 15) had some how leaked therefore are discarded. Vials 7,19 and 20 did not have solid in them, therefore the temperature of the system was lowered to 15C.
[this is not appropriate because you are trying to get room temperature solubilities JCB]
15:50 Centrifuged vials.
16:10 Pipetted 600 ul CDCl3 into NMR tubes.
16:20 Pipetted approximately 50 ul of solvent from each vial into NMR tubes.
16:45 Obtained HNMR of each with 50s relaxation delay (d1),
9A,11A, 12A, 13A, 16A, 17A and 18A
19:00 Solid had appeared in vials 7, 19 and 20 therefore the temperature of the bath had been increased back to 23C.
12:45 Removed vials 7, 9 and 20 from the bath (still containing solid in them) and they were centrifuged for 1min....the temperature of the bath was at 23C, since 13th the bath temperature was not changed. (as far as I know- Khalid)
[what was the temperature of the bath and what happened to your samples when other people were using the bath JCB]
13:00 In to three clean NMR tubes containing 700uL CDCl3 pipetted out 100uL of the supernatant from each vial and obtained HNMR of the solutions with 50s relaxation (d1).
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