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Alicia's Masters Thesis
Open Web Drug Dev.
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Ugi NMR Analysis
To purify crude phenylacetaldehyde by distillation.
Approximately 20ml of
Phenyl acetaldehyde .
was taken in a 100ml round bottom flask and distilled at about 400 mm Hg.
Characterization of 35A
JCAMP Format HNMR
Boiling point of phenylacetaldehyde expected at
400 mm Hg would be 164 C
(based on the reported bp of
195C at 1 atm
), which is consistent with with observed distillation temperature at 167 C. However, the HMR of 35A showed many impurities, suggesting that distillation at a lower pressure be attempted. Also it may be necessary to discard a first fraction. When
both of these steps are taken
, phenylacetaldehyde is obtained pure.
Phenylacetaldehyde could not be purified by distilling under house vacuum (400 mm Hg)
1. 12:12] Approximately 20ml of Phenylacetaldehyde was taken in a 100ml round bottom flask
2. 12:40] A distillation apparatus was assembled, a hose was connected to the in house vacuum terminal (approximate pressure 400 mm Hg)
3. Phenylacetaldehyde was heated using a thermowell until it started to distill. A stable Ubergang temperature (Tu) of 167 C was recorded.
4. 13:20] A drop in the Tu marked the end of distillation. 35A was obtained as a clear oil.
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