Flitting in between playing fallout 2, and separating off the intermediate 1-propionylpiperazine that is the aim of my project. Well half of it. Its a two-step process, an acylation to introduce the propionyl group, then reaction with an alkyl halide plus base for the second step.
No explosion likely, since the acyl and alkyl halides are reactive enough that the substrate need only be introduced to a nitrogen or argon-purged, dry flask, with a stirbar, or since mine appear to have been made off with by the filth, a hard drive magnet, ripped off the backing and smashed with a hammer to snap it in half, the rare earth magnet makes for an effective enough stirbar until I can purchase replacements, or get round to making a better one. and the appropriate halide added, along with a base, in this case, NaHCO3 to absorb the HCl formed as the halide acylates/alkylates the substrate, and stir at room temperature for a few hours.
If the initial project doesn't prove up to scratch, then that will involve heating, 90-100'C for 15 hours or so in 30% sodium hydroxide, which I'd rather avoid, given the time it will take, to use the initial propionyl group as a protecting group, alkylate it, decarboxylate it to give the N-monosubstituted alkylpiperazine and then react it with butyric anhydride and base. Which hopefully can be done without temporarily, because I've been up all night working on it, haven't slept. And the butyric acid byproduct stinks like hell. Well, not exactly, it stinks like vomit, because it is, in fact, the main thing that gives vomit its unmistakeable eau-de-barf. Would rather have used butyryl chloride or bromide for that step if and when it proves necessary (since the propionylated homolog to the piperazine derivative I'm working on should be active itself, but both will be made and tested, since papers differ in their results as to which is the more potent. Either way, getting there. Workup is more tedious than anything actually, since it involves a lot of pouring, decanting, leaving to stand, then separation of a ton of aqueous layer to harvest the bit I'm after, portion by portion. A pain in the arse, not difficult, just repetitive, tedious and annoying when I want to get to the INTERESTING bits.
Speaking of which, time to go attend to the tedious bit. Again. For the third or fourth time:P
