Thursday, March 26, 2009

incredible awesomeness

In my experience it's pretty unusual to have a reaction that not only works well, it actually provides a more pure product than the starting material. I stumbled onto just one of those this week. I have several steps that have been worked out in the route I use and several others I've improved. This little beauty is one of the ones worked out for me, and it seems to be a doozy. I had never put material into the reaction that wasn't clean until last week. I had some residue from crystallizing the starting material that was mostly sm, but had several other spots. I submitted it to the reaction and came out with product that was almost as clean as the ones with clean sm!

To push the reaction a bit, and to try to maximized my amounts of material, I put a really dirty mixture of compounds in. Lane 1 is mother liquor from an 80 run of the prior rxn, lane 2 is similarly from a 40 g run, and has very little sm left in it, and lane 3 is them combined. Probably less than half starting material, but amounts to a wet weight of almost 100 g. I boiled it in acid overnight, and lane 4 shows the results of taking a drop and working it up. Not the most pristine thing, but pretty damned awesome nonetheless.


unadulterated sweetness

7 comments:

Dr. Miller said...

slacker. Do a column.

scientist 1 said...

It's pretty hard to do a column on this scale.

Besides, columns are for pussies.

Mike said...

Speaking of large columns....someone broke "el bomb" again (and it actually wasn't Dr. Miller!).

Jim said...

So that just proves your product decomposes in warm acid slower than the rest.

scientist 1 said...

Actually they all hydrolize and the target can decarboxylate, but not the side materials. In the base wash many side products are removed, while the, no longer acidic, target is happy to stay in the ether.

It's chance as much as proper reaction design. I was just lucky enough to realize it at the opportune time.

Jim said...

That's what chemistry is all about:
getting lucky

scientist 1 said...

Ba-ZING!