I just set up a relatively large reaction (~1.5 mol) using, you guessed it, NaH. Of course I tried it on smaller scale. Of course I'm trying to both bring through material and improve on the existing methods. Unfortunately the preliminary work I had done was a little capricious, so in the interests of time I retunred to good 'ol sodium hydride. I had gotten everything into the flask, I had added all my reactants, I had added a catalytic amount of ethanol to initiate the reaction, I had monitored the gas evolution, and I had even kept a big bowl of ice water handy to cool if necessary.
Everything was going swimmingly, and as I had hoped and expected. After all the reagents were in the flask and gas evolution had dropped significantly, I started to heat for the second stage two hour reflux, and guess what happened.
I've already spent about 2 hours cleaning things that were in my hood like some of the glass that was nearby, and a stirplate. Tomorrow will be the cleaning of the hood itself, and salvaging the last of that reaction. If I'm lucky I'll be able to reassemble my manifold the next day and install it, then I'll be up and running to work all weekend to try to catch up.
Yay chemistry! Yay sodium hydride!
At least no one was hurt.