I arrived slightly later than I would have liked this morning due to the fact I may or may not have had one too many midweek lagers last night.After a coffee (the Nespresso machine in our office has been taking a bit of a hammering this week) and still feeling slightly the worse for wear, I proceeded to start my day’s work. First up was a lithium aluminium hydride (LithAl for the British readership) reduction, a reaction that always works but is also always a pain to do. There just isn’t an interesting way of slowly adding powdered LiAlH4 to a THF solution of the compound in question over the course of half an hour or more and you definitely can’t do it too quickly for fear of getting boiling THF and lithium salts all over your fumehood. Anyway, that reaction was set up and heated to reflux for the majority of the day. I then set about working up some catalyst runs I set up yesterday. I somehow completely failed to purify anything in the first column I did so the other three I have to do were shelved until tomorrow when I’m hopefully in a better mood.
I brought my laptop to work this morning with the intention of spending some of my spare time writing up the experimental section of my thesis. I did not in fact manage any of this today but I did install a piece of software which I had never heard of, Mendeley. Essentially, it’s a reference organiser much like Endnote (a piece of software I never really got on with) which is really user-friendly with a lot of genuinely helpful features. Finally, and best of all, it’s completely free of charge. I recommend giving it a try if you are going to be writing a thesis in the next few years.
Anyway, back to the chemistry. Having spent 20 minutes adding NaOH solution to my reduction, I then proceeded to go through the standard workup. Extract organics into diethyl ether, wash with brine, dry with magnesium sulfate and then filter and remove solvent. Easy right? I first proceeded to find the only blocked sinter funnel in the lab and attempted to use that. I then found the wettest sinter funnel in the lab and looked on in horror as my nice clear solution went decidedly cloudy on its way through the sinter. Drying it again and removing the solvent gave me something resembling pure product which I promptly left on my bench ready for tomorrow where I will probably throw it all over the floor and have to start over. It’s shaping up to be one of those weeks.