While hiking several days ago, I stumbled upon a strange envelope. It contained a strange work of fiction, along with a request to post that story on this site’s forum. Someone named SWIIS had apparently been quite a busy bee. I haven’t been able to figure out what any of it actually meant, but being the good citizen that I am, I chose to relay the information it contained. Maybe one of the bees here can decipher it….
"After several short-cut laden, technique-sloppy reactions (and very predictable low quality, low yielding results), SWIIS had chosen to take a long break from it all.
He reportedly made a triumphant return to the lab. Rumor has it that he was quite successful.
During break time, SWIIS had managed to amass a collection of white 60s, none of which were purchased more recently than March of 2003. He was uncertain as to the presence of O-1 or O-2, so did one JD-Naptha, one naptha, and two MEK boils. The 5 boxes of stock were then extracted per STE. Swiis checked his instrument panel, and saw that his altimeter read 6200 feet above sea level, and all liquids in the STE were increased by 5%. Two recrystallizations using dry iso/acetone yielded an acceptable 10.2g.
To the pristine, corn flake crystals. SWIIS added 7g of MBRP (tragically, the LGRP fairy has not been seen since he was shot down over Juarez), 1.2 of LG I2, and 8ml of dh20. The porridge was then refluxed for 48 hours. SWIIS is in an extremely arid climate, so cooling water was re-circulated. A (.50 cal) ammo can fitted with twin peltier junctions which were subsequently cooled by a takeout fan at 3300rpm, provided a very constant 42 degree bath for the condenser. A very boring 48 hours later, the condenser was removed. Water was added, and the RP hit the flask bottom like a ton of bricks. 3x the volume of the flasks content’s worth of dH2O was added, and boiled (sans condenser) for 15 min. the reaction fluid was 2x filtered through a buchner/filter flask. This was the cleanest, palest reaction fluid SWIIS had EVER seen. The fluid was washed with hot naptha once, and xylene twice. The last xylene wash appeared pristine, so SWIIS decided he was ok to proceed. The setup for steam distillation (per VE’s excellent post) was prepared. He was not about to blow the whole shebang, so he decided to forgo the thousands of square miles in sand that he found out his front door, and he spent the $8 on 100% white pomace (chinchilla bath) sand. He based the eager reaction fluid, and proceeded with the distillation. This time, his condenser was cooled with re-circulated, very cold Ice water (loading ice to run the condenser for a short cooling is acceptable. Loading it over 48 hours is not). Sniff sniff, smile smile. So THAT’S the smell everyone is talking about! The distillation was complete in a hair under 45 minutes. The water in the serparatory funnel was almost completely drained, roughly 6 times the volume of VM&P were added, and the very last of the water layer was completely drained. The np was washed with a nice hot saturated NaCL wash, followed by one cool wash, and a warm wash. The water was extremely clean on the last wash, with no excess of sodium ions. The Muriatic/CaCL wash bottle (with a cotton plug in the neck, just in case) was made ready. SWIIS laughed out loud when he saw the snowstorm forming. He squeezed his little wash bottle until he saw a beaker filled with applesauce. The gassed product had absolutely no yellow tinge. A thorough acetone rinse beat the last layer of NP nastiness from the pile. Curious o see what he was dealing with, SWIIS vaporized a small quantity of his product. The powder burned with no residue whatsoever. Two fairly quick dual solvent recrystallizations were performed with IPA & Acetone.
The 3rd and final rextallization was left to cool at a very slow pace still on the hotplate. 24 agonizing hours later, the crystals were harvested. Beautiful, translucent crystals of balls to the wall crystals were recovered. At final toll, SWIIS was left with a 6.25 g yield.
Read, learn, remember what you’ve learned, and TAKE YOUR TIME would be the moral of this fable."
