Journal of Unpublished Chemistry
The Journal of Unpublished Chemistry, Volume 6, January 30th 2002
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The total synthesis of triethyl ammonium hydrobromide from expensive, difficult to prepare starting materials.
Triethyl ammonium hydrobromide was synthesised in excellent yield from N-tertbutyldimethylsilanyl-4-bromo azetidinone in a single step. Experimental details
PH, UK
pp 1-2
An easier and much more efficient method for the drying of organic solvents.
We were interested by recent reports of the use of ovens for the drying of solvents [J. Un. Chem, p163, 5 (2001)] but, in our hands, these techniques resulted in disappointing yields and elevated levels of capital expenditure. We report here an alternative method of drying which involves reflux of solvents over mild drying agents such as green paper towels or Kymwipes®.
RAK, UK
pp 3-4
On the Classification of Vigorous Reactions.
Did it go 'fizzle', 'phut', 'pop', 'bang' or 'kaboom'? A precisely reproducible reference reaction is described which uses readily available and inexpensive starting materials. By scaling the reaction logarithmically from 10mg to 100g the above range of classifications can be encompassed, bringing to an end any descriptive uncertainty. Workers in Nuclear Physics may find scaling to 10¹¹kg of value, but probably just the once.
ST, UK
pp 5-8
Total Synthesis of Prattleonamine Z, a Selective Cytotoxic Marinated Aromatic Alkaloid when co-administered with Sulfuric Acid.
We report herein the synthesis and biological evaluation of a novel marinated aromantic alkaloid Prattleonamine Z. Preliminary in vitro evaluation indicated that Prattleonamine Z possesses a distinct cytotoxicity profile when co-administered with a molar excess of sulfuric acid. Sulfuric acid on it's own demonstrated the most significant activity against all cancer cell lines tested.
HM*, RK, UK
pp 9-16
Iterative XEM: A Novel Technique for Imaging of Single Protein-Protein Interactions.
Molecules are very, very small, and therefore require specialized instruments for viewing. Conventional techniques such as laser confocal microscopy and inverted fluorescence microscopy lack the resolution necessary for visualization of individual enzyme-substrate interactions, which if possible would enable directed synthesis of small molecule medicines and other drugs.  Here we demonstrate a novel technique, Iterative XEM (Xerox Enlargement Microscopy), for use in optimizing resolution of existing data that may allow nearly limitless magnification.
WCW, WA, USA
pp 17-22
Decomposition studies using deuterated chloroform.
It has been found that due to large numbers of overnight NMR experiments running, compounds that can sit around for days unchanged will decompose whilst waiting in an NMR queue. The original structure can then be deduced from the new spectral data - i.e. that it was the desired compound, and now isn't anymore. A graph of compound importance against likelihood the NMR queue will be full shows a strong positive correlation.
HK, UK
pp 23-26
Suppression of reaction by omission of reagent: hydrogenation.
The reduction of olefins by medium pressure hydrogen in acetic acid was completely suppressed by omission of 10% Pd on charcoal.
CCS
pp 27-28
Suppression of reaction by omission of reagent: oxidation.
Osmium catalysed dihydroxylation of olefins was suppressed by up to 95%, by omission of NMO.
CCS
pp 29-30
Synthesis of Coal From Vitamin B12.
CCS
pp 31-32
Note: Drying of D2O.
We have found that while molecular sieves may be highly effective at removing water from deuterated solvents such as CDCl3, and d6 DMSO, they are suprisingly poor drying agents for D2O.
CCS
pp 33-34

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