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 (https://www.thevespiary.org/talk/index.php?topic=7171.msg43693300#msg43693300)
(TheHobbit: "p-Benzoquinone via H2O2/I2 reaction", Chemistry Discourse)
Post 457743 (https://www.thevespiary.org/talk/index.php?topic=9951.msg45774300#msg45774300)
(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.
a scaled down mm benzo wacker was run with the p-benzo from this post
Post 457743 (https://www.thevespiary.org/talk/index.php?topic=9951.msg45774300#msg45774300)
(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
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...
Did you synth that via h2o2 and i2?
No, that was purchased from a major chemical supply company. I have no experience making it, thankfully. The consistancy of P- Benzo is so fine that upon opening a container of it, fine clouds of it sometimes tend to fill the work space, and your nasal passage, causing burning and triggering my already allergy prone ass into a sneezing frenzy. I couldn't imagine fucking with it anymore than you already have too.
Do some research on it, look in the merk for it's uses, and use the fuckin google search engine, and also http://www.froogle.com (http://www.froogle.com)
Read this thread: Post 374595 (https://www.thevespiary.org/talk/index.php?topic=6479.msg37459500#msg37459500)
(Cyrax: "p-benzoquinone synthesis", Chemistry Discourse)
I am 100% confident that what you have is quinhydrone.
I am also 100% confident that what Midi have is benzoquinone.
The iodine/h2o2 reaction didnt work for SWIM, never went to the quinone, he was stuck at the quinhydrone stage, just like you. It doesnt matter if they are gold or green or dark, those all are quinhydrone, as it look metallic.
Try the V2O5 synthesis from the above thread, 100% easy, not a way to fail, and it give even yellower product than the one from Midi.
You cannot recrystallise quinhydrone to have benzoquinone, you must reoxidize it, that is the only solution, and dont do it with h2o2/i2, it doesn't work.
Ive been trying to use the fuckin search engine but havent really found anything about steam distilling quinhydrone to yield p-benzo.
You're not going to find anything about this procedure, since apparently no bee has ever done this before ;) You've now got the chance to actually contribute something useful to this site, imagine that ;D There are numerous posts about steam distillation of various volatile substances here, and a very good section in the Vogel's 3rd Edition available at:
https://www.thevespiary.org/rhodium/Rhodium/chemistry/vogel3.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/vogel3.html)
Considering the effect of quinone on tear ducts, it would be best to perform such a task with good ventilation :) Any more silly questions and you'll get some bad karma 8) If you can't figure it out with what you've been told in this thread and what's available here and on Rhodium's page, you need to find a different hobby ;D :) ;D
lugh: swim found a synth on google talking about using hydroquinone and KBro3. Not too scientific although. (http://www.uni-regensburg.de/Fakultaeten/nat_Fak_IV/Organische_Chemie/Didaktik/Keusch/p16_ox_hydr_brom-e.htm)
(http://www.uni-regensburg.de/Fakultaeten/nat_Fak_IV/Organische_Chemie/Didaktik/Keusch/p16_ox_hydr_brom-e.htm)
Willy that was the idea. Make the benzo cuz theres no reason to ever take a risk at all ordering anything shady when it can be made, practically otc, easily. Swim read the synth with the h2o2 and i2 and figured it would be the best way to go since it seemed simple and it was discussed a pretty good bit on the hive. Well now swims done the synth exactly as specified 3 times and all swims gotten was quinhydrone. ??? The only thing different swim is doing is the setup. Swims using
a 1 litre erlenmeyer with a 3" octaganol stirbar sittin in a waterbath stirrin at full speed most of the time. Swims usin a clasien to fit the addition funnel and therm obviously. Swims done the synth 2 times regularly, and 1 time at a 2 time scale up. After recrystalizaion the pic above is the same shit swims been getting consistently. The one time swim let the second 3 hour part of the synth stir at 45 degrees for close to 5 hours to make sure everything reacted. Still got the same thing. What the fuck is swim doin wrong? :( Is there any advice anyone can offer swim?
How does the temperature affect the turn from quinhydrone into p-benzo?
C_W is right, the answer to this question can bee found in a thread from the last few weeks, namely Post 464029 (https://www.thevespiary.org/talk/index.php?topic=10017.msg46402900#msg46402900)
(Pimpo: "reflux and reactivity?", Newbee Forum), as well as many other posts about kinetics, and at the beginning of any initial organic chemistry course ::) You are attempting to practice organic chemistry, and to succeed in that pursuit, you need to understand some basic principles, which you could learn by following some of the very helpful links posted in the sticky threads, or downloading Vogel's as suggested :) Thus this thread is being locked, you need to start reading a lot more ;)