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Solubility book (3rd Edn)
To estimate the solubility of the Ugi products UC216-3A and UC216-4A by NMR
The calculations were not considered, since NMR was not found.
The NMR spectrum was not vivid. Hence it had to be aborted.
12:30 Labeled 6 half-dram vials from
1 to 6.
12:45 Placed a small amount of the solute (UC216-3A) in each vial
13:00 Pipetted out 200uL of the six primary solvents in to the vials...methanol Vial #1, ethanol -Vial #2, acetonitrile -vial #3, toluene-vial # 4, THF- vial # 5 and DMSO-vial # 6.
13:20 Placed the vials in the sonicator, temp recorded - 23 C.
13:34 Obtained a picture of the vials in the sonicator with a thermometer. This picture is
13:40 Removed the vials from the sonciator. Temperature recorded - 26C.
13:45 Vials 5 and 6 needed more solute because the solution had turned clear. Hence, extra solute was added.
13:50 Vials 5 and 6 were set on the sonicator again.
13:52 Labeled 6 one dram vials
13:55 Placed a small amount of the Ugi product UC216-4A in each vial.
14:00 Added 300uL of the primary solvents to the vials methanol Vial #7, ethanol -Vial #8, acetonitrile -vial #9, toluene-vial # 10, THF- vial # 11 and DMSO-vial # 12.
14:10 Removed vials 5 and 6 from the sonicator, since these vials had solid remaining at the bottom of the vial of the solvent - temp in sonicator (placed in a beaker) recorded- 25C.
14:20 Placed the vials 7-12 in to the sonicator (in a small beaker containing some water).
14:26 Obtained a picture of the vials in the sonicator with the thermometer. This picture is
14:40 Removed the vials 7-12 from the sonicator and the temp in sonicator (in the beaker) recorded- 30 C.
12:40 Used 25 uL supernatent for Vial #1 and Vial #5.
12:50 Placed Vials #1 and #5 in the sonicator. Temperature recorded-25C.
13:10 The vials were removed from the sonicator. Temp recorded was 26C.
13:55 Labeled and filled vials 216-4A with the solvents, methanol vial#1, ethanol vial#2, Acetonitrile vial#3, tolluene-vial#4,THF-vial #5 and DMSO-vial#6.
15:35 Placed vials 1-6 og 215-4A into the sonicator. Temp recorded was 32C.
16:05 The vials were removed from the sonicator. The temp. dropped down to 28C.
16:10 The vials were later centrifuged for 5 minutes.
16:20 The vials were transfered into clean dry test-tubes which contained 0.7uM Chloroform in it.
16:30 The test-tubes were tested for NMR.
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