Dealing With Unstable Compounds: Part 2

Preparing the post below brought up some great old memories. There was a point in my research career that I really, really wanted to get into phosphaalkene and phosphaalkyne chemistry. The problem was that the entry compound was tris(trimethyl silyl)phosphine [P(TMS)3] which one could buy at that time for $100 per gram. The only option was to make it. The best preparation was refined by Manfred Regitz and his glorious mitarbeiters in Germany. Get this the reaction involved taking pyrophoric white phosphorus (horrifyingly toxic) and heating it in explosively sensitive thf to reflux while slowly dropping liquid Na/K alloy (the liquid metal reduction fire from God) from a pressure equalized dropping funnel (PEDF) all under a dynamic bed of Argon. Once the addition of Na/K was complete you then opened a second PEDF that contained lashing of trimethyl silyl chloride. After the screaming and weeping you then fractionally distill the product to collect the P(TMS)3. I had to hire a post-doc for the one task of developing this reaction in our lab. I later learned that Regitz was so concerned about th potential for disaster in this preparation that he actually had a concrete bunker built in the chemistry department parking lot where his students could do the reaction and if something happened they wouldn't take the chemistry department building out. I had a hard time convincing my post-doc to wear safety glasses.

Anyway the product was air sensitive and would spontaneously catch fire in air and if it came in contact with anything such as cloth or tissue a fire would quickly occur. Needless to say we handled it with the greatest of care.

One day I decided to go to a conference. It was my habit to call back to my lab at dinner time to get caught up on what was going on in my research group. On this one day I was in a phone booth and I called the lab to have my post-doc answer the phone and say the words all supervisors dread ...

"Oh Professor H. it's good that you called ... the firemen have just left."

It turns out that, despite a strict cleaning protocol concerning the glassware used in the P(TMS)3 preparation, a PEDF with a teeny tiny speck of Na/K had somehow made it into our huge rubbermaid ethanol/KOH bath. Hilarity ensued as the teeny tiny speck of Na/K set fire to the ethanol and we immediately had a huge serving of glassware flambe. The column of fire roared up to the ceiling and my post-doc and a graduate student (net cost to me per year ~ $ 46,000) wasted three CO2 fire extinguishers trying to put the fire out. No luck. By now the sides of the rubbermaid container was starting to melt and the contents drip out onto the floor in a scene reminiscent of the movie "Volcano". It was my undergraduate summer student (net cost to me per year ~ $ 0) who understood the situation and found a dry powder fire extinguisher and put out the fire in seconds.

Yes, the fire was out but now every surface in the lab was contaminated with the powder and we would be weeks cleaning the lab. I have no doubt that there are surfaces in that lab that are still contaminated.