Bubbleplate (Hive Bee)
10-18-02 05:17
No 369805
      What IS that white thick crap that almost clogged  Bookmark   

the condenser during post Wacker Ketone distillation?? Swim did all the washes (3 x Sodium Bicarb; 1 x NaCl; 3x NaOH; 1 x dH2O)although he didn't filter. Residual BenzoQ? Sodium BiCarb complex??
SWIM dumped crap and got 150 ml green Alkene anyway! (Better PdCl this time)
Also, is it me or does Ketone smell like "Vic's VapoRub"?
(Chief Bee)
10-18-02 05:43
No 369811
      does Ketone smell like "Vic's VapoRub"? No.  Bookmark   

does Ketone smell like "Vic's VapoRub"?

No. Pure MDP2P has a very weak flowery aroma.
(Drama Queen)
10-18-02 06:19
No 369822
      ?  Bookmark   

What exactly does each wash remove?

3 x Sodium Bicarb; 1 x NaCl; 3x NaOH; 1 x dH2O

sometimes you people forget to do the bicarb and salt wash and just go right to the Naoh.. maybe that is why sometimes ketone polymerizes for bee's who take shortcuts?

Was thinking the only wash that would really be of any use would be the 10% naoh wash, removing the hydroquine, but that assumption is wrong. What do the other washes remove? 

& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.   
(Hive Bee)
10-18-02 06:25
No 369825
      I have also experience the white solid you speak ...  Bookmark   

I have also experience the white solid you speak of.  I believe that is dimerized ketone that sublimates under the conditions of the distillation.
(Hive Bee)
10-18-02 07:26
No 369841
      White Gunk subliming into condenser.  Bookmark   

I seem to recall in one of the MDMA proceedures (maybe Brightstar?) a note that if the hydroquinone isn't removed properly by the washes it will sublime, and cause trouble when it condenses by blocking the column...

Sounds very like what is being described here, no? If thats the case the washes weren't sufficient to remove all the waste quinone.

(Hive Bee)
10-18-02 16:38
No 369933
      I Don't Think That Gunk Is BenzoQ  Bookmark   

As it doesn't smell like BenzoQ. I HATE the smell of BenzoQ as it makes me ill, and can detect minute traces. I'm leaning more towards what lab_bitch said: "dimerized ketone that sublimates.." or something else.
Some testing of it is called for.

The "Vicks VapoRub" smell I alluded to was for raw Ketone.
Subtle odor, not strong or over powering. Will have to see if it disappears or changes when re-distilled.
Thanks all!
(Hive Bee)
10-18-02 19:18
No 369972
      Mystery Gunk Identified - Sort Of....  Bookmark   

20 ml of the white condenser clogging "Gunk" was isolated and added to 200 ml dH2O and kept overnight at 10 C. Next day the "gunk" had turned into brownish globules of oily material, which floated in and near top of H2O (NOT sinking). Suctioned and filtered oily material to get approx. 15 ml of clear deep Red-Brown-Greenish oil. Oil has intense "Vicks VapoRub" odor, and apparently is source of odor in Ketone as mentioned. Small amount of charcoal particles added to oil caused spontaneous formation of small flat angular "waxy" crystals. In addition, when test tube of oil was shaken, small amount of material on sides formed waxy deposit very similar to original material clogging condenser. Oil is soluable in DCM, acetone, etc.
So... it appears that this material is indeed some sort of Ketone and/or Ketene by-product from the Wacker reaction.
Wish I had GC and IR at my disposal to see what this stuff really is.
(Chief Bee)
10-19-02 00:30
No 370037
      is it soluble in 10% NaOH, but insoluble in 10% ..  Bookmark   

is it soluble in 10% NaOH, but insoluble in 10% HCl? (if it is, it may be hydroquinone or a piperonylic acid)
(Hive Bee)
10-19-02 00:33
No 370039
      why don't you do a bisulfite test on it to see if ...  Bookmark   

why don't you do a bisulfite test on it to see if it's some kind of ketone?

Who is that masked man?
(Hive Bee)
10-19-02 00:35
No 370040
      Vicks VapoRub odor  Bookmark   

Some pinacoles smell like that, could a pinacole (as a byproduct from impurities etc.) have formed during your reaction?

Quidquid agis, prudenter agas et respice finem!
(Hive Addict)
10-19-02 06:04
No 370116
      Camphor?  Bookmark   

  Could be camphor... which is what comes to mind...may be in your particular batch of precursor... known to be in sas oil at low levels, depending upon source...

Here's labtop's data from utsfe
pinene.......... 2-10% Bp= 154C at 1 atm
phellandrene. 2-10% Bp= 175C at 1 atm
d-camphor.... 0- 5% Bp= 204C at 1 atm
safrole.......... 80-90% Bp= 234C at 1 atm
eugenol........ 0-10% Bp= 252C at 1 atm

 The phelladrine, which does not have a m.p. in any source I've been able to locate, seems to freeze at around 47-41 deg. Farenheit. I am waiting for my fridge to adjust it's temp down so I can do a reverse melting point test by taking all of the apparatus out of the fridge and checking it as it thaws out...

Infinite Radiant Light - THKRA
(Hive Bee)
10-20-02 04:54
No 370379
      Did Some More Testing  Bookmark   

It did precip some with bisulfite, so certainly some of it is ketone like; however, the waxy "semi-crystals" and some of the liquid remained.
I left (10 ml)the remainder of it out at room temp, and 24 hours later it did darken and appears to have decomposed somewhat. However the odor is still strong.
Camphor - well, the more I think about it, the more I think that MAY be a component too. It did come over well before the ketone at about 70-80 C. (29.8 inches vacuum). The saf. of this batch was from the first "home distilled from roots batch" of oil, and that it wasn't distilled that carefully as later batches with perforated plate and special Vigreux's.
All new oil will be double distilled through the vacuum jacket columns with a keen eye on the temps!