Recrystalization of Meldrum’s acid from acetone – Prepping for the pilot reaction

So the reagents for the synthesis are finally almost all here, last one should arrive today.  While we’ve been waiting for things to arrive we’ve been trying to get the NMR at school back up and running.  A lack of nitrogen for the high pressure tank kept me from running any samples today though sadly, so will have to wait until next Tuesday to see how well it works when the gas is delivered.  It’s sad to see such a nice machine (Varian 300mhz) sit in a dark back room so we’re trying to give it a purpose to come back to life!

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From a granular yellow/white powder to pretty nice crystals, the first pass will be enough to test the next step which is acylation of the Meldrum’s acid with an acyl halide.  The conditions call for slow addition of pyridine to the Meldrum’s acid and acyl halide in DCM under inert conditions.  We’ll see how that goes…

 

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