Author Topic: p-benzo pics... no bees want to see? =(  (Read 4800 times)

0 Members and 1 Guest are viewing this topic.

homeslice

  • Guest
p-benzo pics... no bees want to see? =(
« on: October 15, 2003, 07:38:00 PM »
Swim recently synthed some p-benzo from h2o2 and he asked me to post these photos for him. Other pics on the hive dont resemble this at all. But when described by text they match the description. These are after recrystalization and drying.










Swims just a little concerned about it because he spent hours reading p-benzo posts on the hive and has yet to see a picture that looks like this.  :(  So what do the bees think?

GC_MS

  • Guest
My commercially obtained pure 1,4-benzoquinone
« Reply #1 on: October 15, 2003, 08:22:00 PM »
My commercially obtained pure 1,4-benzoquinone is yellowish. I have purchased the same substance from SA and theirs turned out to be greenish (and contains an impurity; I don't know which one, but it was hard to remove it from certain reaction mixtures).


homeslice

  • Guest
so?
« Reply #2 on: October 15, 2003, 08:46:00 PM »
GC_MS: so whaddya think?  ;D

Vitus_Verdegast

  • Guest
quinhydrone?
« Reply #3 on: October 16, 2003, 02:11:00 AM »
That is probably quinhydrone, these are green crystals with a metallic shine.
Is it possible to oxidize hydroquinone to p-benzoquinone with just H2O2? Any ref you got for this? When I tried it it gave are really darkgreen, almost black solution of the charge-transfer-complex quinhydrone.

If you oxidise this further with a suitable oxidation agent, you'll get p-benzoquinone.

Quinhydrone may very well be the contaminant of commercial lightgreen benzoquinone.





ChemoSabe

  • Guest
Chem Porn Revival
« Reply #4 on: October 16, 2003, 02:53:00 AM »
Nice images. Sometimes such imagery is referred to around here as chem-porn and I hope you and other bees continue to produce and show more images such as this.

Much like sex oriented porn, seeing it sure beats the hell out of just reading about it.


homeslice

  • Guest
hmm
« Reply #5 on: October 16, 2003, 03:52:00 AM »
Chemosabe: Thanks. I wish the hive had a place to upload photos to. I think if it did in the future more bees would display their work maybe?

That was the exact reason why i posted pics to make sure they weren't quinhydrone. They are definately NOT black. The crystals DEFINATELY look like the color of gold. Id say it really resembles fools gold, since swim has seen quantity of this. The color is hard to see in these pics as they were taken with a cell fone  :)
Its not just h2o2 its 35% h2o2 that was ordered by swim from a chem supplier.

Some refs: The original synth is on Rhodiums site but its also reiterated in this post by overclock. Ive also seen overclocks version of this synth referred to in other posts.

Post 257969 (missing)

(overclock: "p-benzo via H2O2 etc ...", Newbee Forum)

Post 436933

(TheHobbit: "p-Benzoquinone via H2O2/I2 reaction", Chemistry Discourse)

Post 457743

(blaaky: "p-benzoquinone via h2o2 results", Newbee Forum)
     <-- now this is the post with one of the pictures that worried me into thinking that i fucked up.  But then i did the synth again and got the exact same results with about the exact same yield as prescribed via overclocks method.

Its tough as a newbee chemist to look at something you made and say that its the right stuff. Like i want to believe that that is 100% pure p-benzoquinone, but then i read on here posts that have conflicting ideas on what p-benzo should look like, smell like, what color it should turn when its placed on ur skin. And then reading conflicts like this makes me wonder if swims work is absolutely wrong because obviously these bees posting these conflicting reports have more exp. than swim.  :(
I got some reassurance in swims work though when I stumbled upon a post on the hive that was written by an experienced bee, I cant recall whom (shouldve bookmarked), that mentioned how newbees can look at safrole and see that it distilled at the right temp, it refracts like, it smells nice and pleasent and every other thing that safrole should be... and then STILL doubt their work. Like swims p-benzo seems to be bright yellow crystals that burn your eyes and nose just going near them but then it makes me wonder if swims just in disbelief because hes a newbee and doesnt have a shred of confidence.  :(  I dont know just my two cents buts its prolly more like newbee rambling to many.

Vitus_Verdegast

  • Guest
steam distill if you really want to be sure
« Reply #6 on: October 16, 2003, 04:55:00 AM »
That was the exact reason why i posted pics to make sure they weren't quinhydrone. They are definately NOT black. The crystals DEFINATELY look like the color of gold. Id say it really resembles fools gold, since swim has seen quantity of this. The color is hard to see in these pics as they were taken with a cell fone

Yup, it is sometimes difficult to judge the color from pics, as they seem to always differ somewhat from the actual colors. That is why judging from your first pic it seemed dark metallic green to me.

Its not just h2o2 its 35% h2o2 that was ordered by swim from a chem supplier

Not what I meant, I was wondering if you used H2O2/I2 or only H2O2, since you didn't specify that.

Like swims p-benzo seems to be bright yellow crystals that burn your eyes and nose just going near them but then it makes me wonder if swims just in disbelief because hes a newbee and doesnt have a shred of confidence.  I dont know just my two cents buts its prolly more like newbee rambling to many.

Well, that doubting when performing reactions the first time is only normal. It's only from experience you learn to be more confident in what you do is right. The way you describe it, it sure sounds like p-benzoquinone.

Or: You could steam distill it. Just add the crystals to enough water and distill. Quinhydrone will dissolve in boiling water, and the quinone will be carried over. This way you should get very pure p-benzoquinone.


wolfx

  • Guest
p-benzo appearance
« Reply #7 on: October 16, 2003, 05:02:00 AM »
From the Merck Index, 12th edition :

"Yellow monoclinic prisms"

I agree, the color should be bright yellow, looks like hydroquinone but yellow. I think usually we see a bit green-yellow because of quinhydrone ( ? ) contamination. Looks like you have a lot of impurities in your product.

I have been trying to make / purify p-benzo via dichromate ( SpiceBoy ), but I have had a lot of trouble also. The final product, after filtering, has a lot of Cr impurities and water, looks muddy, very green ( pea green ) and differently than pure p-benzo, is VERY water soluble. The green color is due I guess to Cr2O3. Yields are easily 140 %, what tells you there is a lot of impurities and H2O. I have tried to purify with DCM, and the final product superficially looks OK, nice yellow, just a hint of green color, dry powder, but there seems to be some residual impurity remaing or generated when using DCM. Twice I had strange results with the Wacker, lots of impurities, solid black tar, low yield, usually 30 % or so. In another occasion similar black tar showed up mixed with the freebase when xtaling, but washed away with acetone. Low yield, though. Benzene seems to work better but yields are low, also difficult to distill out when p-benzo concentration starts to increase. I had to use aspirator vacuum for the DCM as well as for the benzene.

If using the dichromate method, best technique seems to be to dry it WELL after filtering, let it stand inside a glass container with drierite for a few days, might have to change the drierite once or twice. Don't try to purify, use as it is and use a slight excess. I hit 65 % ketone yield on my first try, never was able to repeat that.

Also, black tar etc. never showed up, only when I tried to purify with DCM. Low yields with the Wacker, though.

I think the H2O2 method is a better deal, but I have never tried it myself. I have heard other bees have got quinhydrone instead of p-benzo, it might be very well what you get.

If you can buy it you will avoid a lot of headache, but be careful. I have ordered it once, they call me back and said they needed a statement from me or my company telling them what I was planning to use it for. I said I would do it, then called them back again, said please cancel it, they said OK, no problem. This was about two years ago.

Other bees comments will be very welcome, I have high interest in this topic.

homeslice

  • Guest
so whats the verdict?
« Reply #8 on: October 16, 2003, 05:20:00 AM »
I agree, the color should be bright yellow, looks like hydroquinone but yellow. I think usually we see a bit green-yellow because of quinhydrone ( ? ) contamination. Looks like you have a lot of impurities in your product.
Ive read that quinhydrone is dark colored, almost blackish. Theres nothing in there that is anyting but gold colored. When swim takes out about 2-3 crystals of that and applies a nice light to them swim can easily tell that they are 100% gold colored, kinda bright yellow. Swim followed the synth exactly word for word exactly and sat there the whole time to make sure everything went well. Twice Swim got the exact same thing, which makes swim think he did it right but swim would feel alot more reassured when a senior bee says "yes homeslice thats p-benzo and it looks great"
So whats the final verdict here? P-benzo or quinhydrone or p-benzo w/ quinhydrone? Should i proceed to the wacker with this?

Whats really on swims mind is that when he does the wacker, if he gets poor yields, he doesnt want to turn around and blame his benzo and then be pissed off at himself for not getting a 100% reassurance that it was benzo to start with...   ;D

wolfx

  • Guest
To go or not ?
« Reply #9 on: October 16, 2003, 05:47:00 AM »
If you have only quinhydrone as contaminant, I don't think it is a serious problem, just use a slight excess of p-benzo and you would be OK. But, I suppose quinhydrone contamination would make your p-benzo kind of green-yellow, maybe a lot green, and should be still kind of nice, dry, powdery. You said it looks gold colored, that I don't understand.

I guess you might get a low yield with the Wacker, but I don't feel like I an experienced enough to tell you go for it or not. Up to you, maybe ask some of the more experienced guys. Please post your results, I am interested in the H2O2 method as well.

Good luck,

W.

chilly_willy

  • Guest
and that color is..?
« Reply #10 on: October 16, 2003, 08:02:00 AM »
Im not sure what the big question is regarding this.  Is it yellow or isnt it?  It looks very black green in that picture.  Pure benzo is canary yellow--as in post-it-note yellow; smiley yellow; legal pad yellow.  Over oxidized benzo, or benzo that has been left out in air turns green. If its not bright yellow its not pure.  Why dont you inquire on how to get it nearly reagent pure bright yellow?  In one of my posts- I got quite descriptive on how to do this. How long, and at what temperature was it reacted at? What were your reactants, and at what ratios?  Crystallization procedure?? Ask these questions and then post the pictures of your blindingly bright, no questions asked benzo.
This reaction is great once the kinks (if there are any) are ironed out...


blaaky

  • Guest
just to chime in...
« Reply #11 on: October 16, 2003, 08:46:00 AM »
a scaled down mm benzo wacker was run with the p-benzo from this post

Post 457743

(blaaky: "p-benzoquinone via h2o2 results", Newbee Forum)


The resulting ketone looks and smells good, amination pending.
Note: previous benzo wackers were run with the pea-green benzo purchased from a photographic supply and had positive amination results.

blaaky


homeslice

  • Guest
Its all yellow. There is no green.
« Reply #12 on: October 16, 2003, 04:40:00 PM »
Its all yellow. There is no green. Im going to try to borrow my friends digital camera later today to get better pics of it.

Why dont you inquire on how to get it nearly reagent pure bright yellow?
Ive been looking everywhere for an answer to this!
It was reacted at the exact temperatures that overclocks method says. Swims reactants for the first time were a 1x scale of overclocks method and the second time swim did a 2x scale with the exact same results. Swim recrystalized with 91% almost boiling ISA. Let it cool to room temp. Placed in fridge. Placed in freezer for an hour. Then vacuum filtered and rinsedwith ice cold ISA. I'd get into more details now but i got 2 classes to go to  :(

My two roommates agree with me that the color is definatly the color of gold.
Ill try to dig up a digi camera later.

chilly_willy

  • Guest
Re: clean benzo (Rated as: good idea!
« Reply #13 on: October 16, 2003, 06:46:00 PM »

clean benzo
(Rated as: good idea!)     Bookmark  Reply     

First of all this reaction can be scaled up if you are prepared to drop the flask in cool water when things start to heat up.. Also- It is well to let the reaction continue to just slightly boiling for some time. When you think you are ready to crystallize drop the whole flask in the freezer for an hour or so until you get quantitative amounts of YELLOW benzo.  Take everything over the the buchner and suction filter.. being sure to use plenty of ice cold alcohol to wash everything well.  Use saran wrap as a dam to get the last of the liquid out.  At this point your benzo should be yellow with a hint of red...canary yellow if you washed it well.  If it still has a red tint/flecks..you can recrystallize from denaturated, methanol or even water to get perfectly bright yellow crystals.  Remember as well that you can use methanol, denaturated, or isopropyl for the reaction solvent.  Afterwards put your damp Xtals in a shallow tupperware container within a larger one with CaCl..and in a few hours you will have nice large bright Xtals that dont huff and puff when you drop them in that giant 5L...







homeslice

  • Guest
recrystalize
« Reply #14 on: October 16, 2003, 08:27:00 PM »
Swim chose ISA to recrystalize because another bee said it bee ok.

Chilly can u post a picture of ur p-benzo? Or can anyone post a picture of their p-benzo? Swim needs something to compare his to. All the benzo posts on here talk about how its either old or photo-grade benzo. Swim needs a picture that is good p-benzo displaying these bright yellow crystals that swims heard so much about.

homeslice

  • Guest
Ok new pic
« Reply #15 on: October 16, 2003, 10:24:00 PM »
New picture. There are other ones but they are too large. This was a much higher resolution but swim had to shrink it so it didnt take forever.



MUCH better higher resolution picture. Now.. can someone give swim a definate ID on what the fuck it is? ;D  Is it good to use for the wacker or is it going to hurt my yields significantly
See why i referred to it as gold colored now?

Midi

  • Guest
an idea..
« Reply #16 on: October 17, 2003, 01:00:00 AM »
Dunno what you got there, but I wouldn't use it.

As far as I know, P-Benzo is not listed, nor watched in small amounts, and I have seen it being offered recently in the US. I am not saying you should buy some, but really you should. It doesn't look like you have more than 500g there, and 500g amounts aren't going to raise any eyebrows. Recently, a friend of a friend sucessfully imported 5kg, not a single problem. If you have good safrole, it shouldn't be wasted. Get the right stuff. What you have may work, but yield would suffer so much it wouldn't be worth the wasted paladium.


homeslice

  • Guest
im confused then what does p-benzo look like
« Reply #17 on: October 17, 2003, 01:04:00 AM »
I did the synth twice with all lab grade chemicals exactly as it says and got the same results? Is the synth wrong then if thats not p-benzo?

Midi

  • Guest
P-Benz Pic
« Reply #18 on: October 17, 2003, 01:21:00 AM »



wolfx

  • Guest
Looks OK
« Reply #19 on: October 17, 2003, 01:30:00 AM »
This one looks like the real McCoy.