When I finished with DMF wacker...I knew something didn't smell right, but decided to give it a whirl in a 2.5x al/hg and ended up after gassing...with this yellow solution...and yellow nasty crap collecting on the bottom of that beaker and on the dispersion tube...not much...but just a nasty yellow gooey semi-solid...kinda like a juicy booga or something...
Anyway here is the reaction I tried if anyone can see something I did wrong, please comment...also, if anyone has any comments on what to do with the yellow crap/toulene mixture...let me know PLEASE...? Maybe an A/B? I have heard/read of many bee's attempting wackers...swearing they had ketone...than after an al/hg...got nothing.
Here goes:
1) In a 4L Filtering Flask placed 1150ml DMF, 7.5g of pdcl2, 41.25g of CuCl, and 170ml of dH2O. I let this stir uncapped on high for 3 hours.
2) Added 750g safrole. Capped up with rubber stopper and large wire ties...along with a little duct tape.
3) Attached o2 tank with high pressure hose to vac adapter and purged vessel 3x. Pressurized to 33 psi and turned stirring on high.
4) At this point I cannot say how much pressure dropped in total becuase of the fact that half way through I found a small leak. But I was checking it every 20 min and the pressure seemed to drop dramitically every time, until the end. Within one hour the flask was certainly warm...and within 2 hours was hot. Here's where I may created a problem...at the 220min mark...I fell asleep...stupid me...and when I awoke 7 hours later...all the pressure was gone from the flask. Could this have been a problem?
5) Added 1250ml 5% HCI solution...let oil fall to the bottom.
6) Extracted mixture (without sep raw oil first) 3x with 250ml DCM.
7) Washed DCM extracts 2x w/750ml NaBicarb
![Cool 8)](https://thevespiary.org/talk/Smileys/default/cool.gif)
Washed DCM extracts 1x w/750ml NaCl
9) Dried DCM with 140g of mag sulfate
10) Filtered and distill DCM
11) Frac Distilled ketone. Between 100-130C I got what I thought was ketone. And I know that is a large gap in between temp, but there was really no noticeable fluid change...I imagine this could be another problem, right? I will frac distill what I have left to see if I do, for sure, get two fractions. BTW, I ended up with 430g supposed ketone.
NOTE: Another thing I noticed while reading from my Notebook...is where I noted that I added the water in the beginning of this synth, I (in the notebook) wrote down 670ml...which would have been what was required in a 3kg DMF Wacker (per LT)...but I do not think that I would have been that careless to add that much water, I knew that the amount was small (167.25 ml)...although, anything is possible. I have a habit of writing down steps before they are completed. So, with that, what would have happened if I actually did add that overdose of water?
Thanx in advance.
peace.
DEM
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