Post 235232 (https://www.thevespiary.org/talk/index.php?topic=7242.msg23523200#msg23523200)
(Rhodium: "Re: Tasting E freebase oil..", Chemistry Discourse)AWESOME i thought and made the LAH for 30 grammes of nitrostyrene. After the LAH was put in the THF i discovered that the magnet was left in the nitrostyrene, which was a whopping 8 grammes :(
LOL! Join the club, my friend! Leaving the stirbar somewhere in my crystalline mass is one of my very-often made mistakes. The reason why I make this mistake so often is because I usually do small-scale synthesis, using tiny stirbars that easily disappear in the crowd of glistering crystals. Especially when I'm doing nitrostyrenes... And no, my latest reported yield of 80% 2,5-DMNS was WITHOUT the stirbar :P
THIS (https://www.thevespiary.org/rhodium/Rhodium/pdf/thf2gbl.pdf)
(https://www.thevespiary.org/rhodium/Rhodium/pdf/thf2gbl.pdf) procedure SWIM read you have to take care of the excess bromine form in situ. Fine by me said SWIM, left the contents stirring, plugged a hose for driving fumes out the window and went to watch some TV. Some hours later he came back to his tiny turned-into-a-lab bathroom to find out it was filled with bromine gas. Damn...opened the window and turned on a fan to vent the place AND stayed in to clean up the mess on the working table. Bad idea. It wasn't immediately but some 30sec. later, SWIM could barely open his eyes and had this burning sensation in his mouth. Run away and put his head under the faucet with cold water running at full throttle on his eyes and face. That's when the telephone rang. It was SWIM's friend to chat up a while. Bad, bad moment for chatting.