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Where’s the Spin?? December 20, 2006

Posted by thwalls in Blogroll.
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Still nothing new unfortunately.  I’m hoping that after this examination that’s coming up in February I’ll devote a bit more time to the endeavor that this is by bringing up some new and novel chemistry…but at the moment I’m trying to make sure that I have enough sources for my Candidacy Research paper.  I’m hoping to get this done by the end of the week so that I can get some people started on my reviews, but we’ll see how that goes. 

Either way, I’ve found some novel Vanadium chemistry that should yield better results for my cyanation of an aryl ketone.  This is some of the work with the Vanadium triflate catalyst that seems like it can do anything but make you a sandwhich while the reaction is running.  Apparantly you just take some oxo-vanadium sulfate, and impregnate it into a dowex ion exchange column.  You then pass through it a solution of hot 1 M triflic acid and presto chango, you get vanadium triflate out the other side which can then be used directly in your reaction that is high yielding and exceptionally easy to work up.  The vanadium catalyst is actually very water soluble and thus can washed out, leaving only your product and any remaining starting material, so hopefully just two spots on the TLC plate…well actually I’m hoping for one…

Our lab also purchased a new 400 MHz Varian NMR which we’ve been using like crazy, especially after not having access to one for over 3 months.  So for some reason you’ll be using it and the guage that measures your NMR tube spin will spontaneously drop to zero and your nice flat base line turns into thick-sliced bacon as your peaks become uber fat…so not too happy about that.

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Comments»

1. Tex - December 20, 2006

Spinning can be a pain. Assuming that there is no problem with the air supply (check pressure is adequate), check that the spinner is not dirty (or the checks around the top are not dirty). Another common problem is that diry gets into the probe, particularly where the spinner sits, and so it may need cleaning. Our NMR guy has made his own huge Q-Tip for cleaning the probe without removing the probe.

2. thwalls - December 21, 2006

I like the Q-Tip idea. But we just got this NMR, and it’s not even registering at the instrument at all. Apparantly we were told that we have to reset the controller any time this happens. But that just seems tedious. Especially with the cost of the darn thing. It’s like an old Mazda that needs to be restarted after it stalls in traffic…


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