Hey guys, SWIM would have posted sooner, but SWIM was at GF's house all weekend enjoying the fruits of his labor.
SWIM is not so sure the pills were neo-gakked (shaddap) after all.. Or perhaps SWIM inadvertently got rid of it somehow..
The former would be more likely.. But SWIM was under the impression that pretty much any pill (esp. the 120's) with a >;;;;2006 expiration date would have the new gakk.. Most of SWIM's pills had >;;;;2006 exp date.
So just for the hell of it SWIM will write a very informal and likely innacurate report on this latest reaction of his.
Well you know the details of the reaction itself except it's length, which was about 30 hours (minus a few hours from the various problems that occurred, SWIM would guess).
SWIM really wanted to let it go the full 48 hrs, but was really pressed for time.
Ah there is actually another detail that may be of interest; for the last 6 or 7 hours of the reaction (which SWIM reminds you, in case you forgot, was carried out in a lava lamp) SWIM switched the 40W bulb for a 60W one.
The temperature on the surface of the bulb was approx 140C.
SWIM is sorry, but he does not know the temp of the rxn fluid itself, nor does he know how to derive it from the temperature value of the surface of the bulb. If SWIM was to pull a value out of his ass, it would probably be 130C, but he has no reason whatsoever for thinking that. SWIM just has a gut feeling.. Or perhaps SWIM should lay off the baked beans (amongst other things)..
Anyway, SWIM did this because he knew that he would not be able to let it go 48hrs, and figured it could help a lot to raise the temp in the flask to speed it up a little. SWIM can't really say whether this worked in his favor or not.
SWIM became aware of some past discussions on rxn temp, and its effect on the presence of undesirable compounds in the end product. It was too late to turn back really, so SWIM said "fuck it".. SWIM was then made to wash his mouth out with soap.
Oh BTW, SWIM did not "reset the timer", so to speak, on addition of new precursors (well, just I2 really) as was suggested by ware. Again, time was scarce.
SWIM also read about using UV and whatnot to help the rxn.
SWIM was in an experimantal mood, so he set up a small fluorecent light to shine in the vessel. This continued for a couple of hours, then the rxn vessel was placed in full sunlight on the windowsill for about 4 hrs until the end of the rxn.
The sunlight seemed to have quite a noticeable effect on the rxn, which SWIM could only describe as an increase in vigor.
Post reaction, SWIM washed the living fuck out of the rxn fluid, on account of the vast amounts of I2 left in there after filtering a couple of times. SWIM started with about 4 or 5 xylene washes.. SWIM didn't keep count unfortunately.. SWIM is starting to see the value in recording details in a notebook as one proceeds.
After the (now crimson) xylene washes, SWIM washed with TCE, which turned pink and caused much annoyance by being heavier than water.
This was followed shortly by a couple more xylene washes, as the color of the rxn fluid was still somewhat darker than considered ideal, and finally a couple of hot naphtha washes.
Btw SWIM WAS aware of the boiling trick used by some to get rid of excess I2, but SWIM only thought of it AFTER diluting the fluid with hot dh2O.
SWIM's A/B was in the form of a kerplunk type thing with naphtha as the NP. SWIM did 2 pulls. Washed twice with plain dh2o.
SWIM titrated, and ended up with some excellent (by SWIM's standards) product. It is sparkly as hell, and just as potent (hence this giant rambling post). Seems pretty clean to SWIM, but what does SWIM know.. SWIM has yet to rxtal due to time constraints, but will be doing that either tonight or tomorrow.. Will let you know.. whether you like it or not..
Thanks to ware and shawtey for the tips..
Lata fewlz