10/09/2006

"if we knew what we were doing, it wouldn't be research"

The past bit of research I've done has not been terribly productive. There's one reaction I've been working on. Just one. It takes about two days or so to run and another day or two to quench. Then, there's a nasty black emulsion, you can't see the phase separation at all, and even after another day of just sitting there it hasn't broken. (Finally I got a little impatient and filtered it. That worked wonders.) GC/MS'd it: Teeny tiny bit of desired product. Lots of either starting material or something very very close to desired product (same molecular weight). Lots of completely unusable crap. Needless to say, I'm glad to be able to avoid running this through silica, since the TLC looks like a PCR reaction gone horribly, horribly wrong. I am less than thrilled to have already run this more than once.
Especially after today's revelation from the boss: "Hey, look at this guy's lab notebook! He used a completely different approach and it actually worked!"
Perhaps it is a curse.

4 comments:

Andrew said...

When getting with a reaction in the first time some experences tell me that you can get better results by repeating with no conditions changed. First-time trying is always failing. In fact some conditions do change when you repeat. You more carefully wash the flask, watch the temperature and quench the mixture something like that.

Ψ*Ψ said...

well, yeah, i admit i screwed up when quenching it the first time. but what i did for the deoxygenation didn't work anyway, so it doesn't matter too much. :)

gaussling said...

Was there a major product or was it just a dogs lunch?

Ψ*Ψ said...

Absolutely all junk. I only got it to (finally!) work a few weeks ago...