URSS: we’re halfway there…
The weeks have flown by, and this week marked the halfway point in my summer project. I’ve really enjoyed the experience so far and I’ve learned a lot- I’m a lot less nervous/clumsy in the lab these days so surely that’s a good sign!
Up until this point I’ve been making a lot of the compound I mentioned in a previous blog. I’ve had to repeat the same reaction so that I have enough crude product to be able to purify in the next step and still get a decent amount at the end. While doing the same reaction over and over again did get a bit tedious, comparing how much I struggled to do it the first time to how quickly I can get it sorted now has meant I can see my confidence in the lab growing!
I’ve also been working on some resorcinarene chemistry, where I’m basically making a bucket-like molecule which could eventually have interesting applications in catalysis and C-H bond activation. So far, I’ve made a macrocyclic compound with four quinoxiline walls surrounding it, and I’ve gradually been isolating the same compound with different walls removed. Over the course of my project I’ve got samples of the two isomers with just two walls (the ‘bis walls’), and the version with three (the ‘tris-wall’). The molecule we’ve been interested in is the tris wall, so for the last few weeks I’ve been trying to separate this particular fraction out of all the other samples. To do this I reacted the starting ‘tetra-wall’ compound in reaction conditions that favoured the formation of the tris-wall over the two bis, and then used a separating column to remove the compounds I didn’t need along with the single wall that was removed.
Here are some pictures of my reactions that I took right at the start of my project. While here they don’t look particularly pretty, they’re all shiny white crystals now!
Before starting my URSS I had only used a separating column once or twice in undergraduate labs, and since they tend to take a long time, neither of them really worked in the few hours I had. But now I’ve had the chance to do a few columns properly, and actually understand how the technique works. Separating all the different fractions has been a bit of a pain to be honest, especially when the chemistry building’s fire alarm went off twice in one day and I had to leave my experiment. The annoying thing about using a separating column is that once you start the solvent running through to separate the fractions in your material, you can’t really stop it, so having to leave it twice in one day wasn’t ideal! However, nearly five weeks later I’ve got some pure(ish!) tris-wall that I can do some reactions with. The idea now is to do some organic reactions to attach a molecule to the tris-wall in the space where one wall has been removed. The current step I'm working on is meant to take 3-15 days to react, so I'll just have to wait and see how it turns out!
However, even if my project doesn’t work out as well as we hope, I would still have no regrets about giving up most of my summer to work in the lab! It’s been a great experience, the people in the research group I’m working in are all lovely, and I’m looking forward to the next three weeks. It’s really opened my eyes to the world of research, and made me consider career paths that I hadn’t thought of before.