Hello Maybe all of you out there surfing the tubes on the interweb can help me out. I have a DIY project set up and i will be doing this project as an
individual not under a university. I am trying to find a site to obtain 2,4 dinitrophenol but sciencelab is the site that i can find that sell to
individuals but i have been ripped of by them before. Any help on alternative sites?undead_alchemist - 22-12-2007 at 07:05
Lets just say the shipping and hazmat fees would cost more then the chemical.
And there are other places that do have access to it. but because of the fees, its a loss item or has a very high price from any secondary sellers.Sauron - 22-12-2007 at 07:15
Why not make your own 2,4-dinitrophenol?
This not difficult.soto3330 - 22-12-2007 at 09:53
Quote:
Originally posted by Sauron
Why not make your own 2,4-dinitrophenol?
This not difficult.
My project didn't involve making 2,4-dinitrophenol. willing to learn. Care share any links for good straight forward information on doing sochemrox - 22-12-2007 at 10:46
ScienceLabs is very very slow .. often don't answer phones and have to pester them with faxes and eamils to get any kind of response. If you want to
experiment with chems get established with one of the mainstreams it will be worth it in the longrunMagpie - 22-12-2007 at 11:10
Too bad you didn't UTFSE on this site before attempting to deal with sciencelab.com:
Originally posted by chemrox
ScienceLabs is very very slow .. often don't answer phones and have to pester them with faxes and eamils to get any kind of response. If you want to
experiment with chems get established with one of the mainstreams it will be worth it in the longrun
um ya i was told there was a backorder after i order from them and they told me 7/8 weeks. We are now going on week 17.. At this rate i wont get
anything from there for about 2yrs.soto3330 - 22-12-2007 at 11:20
Quote:
Originally posted by Magpie
Too bad you didn't UTFSE on this site before attempting to deal with sciencelab.com:
At this point have filed with the BBB... too bad i didn't see that.
Making 2,4 - dinitrophenol sounds possible any help would be appreciated or link to site to just get the 2,4-dinitrophenol would go with a big well
known place but they don't sell to individuals.MagicJigPipe - 22-12-2007 at 14:41
For those of you who don't like abbreviations or don't live in North America, BBB stands for Better Business Bureau.
From Wikipedia:
Quote:
The BBB states its purpose is to act as a mutually trusted intermediary between consumers and businesses to resolve disputes, to facilitate
communication, and to provide information on ethical business practices.
Sauron - 22-12-2007 at 16:29
2,4-DNP is usually made by dinitration of chlorobenzene and then fusion with NaOH in an autoclave and liberation of the dinitrophenol from the sodium
phenoxide.
I'd be curious to know the nature of your project and why you need 2,4-DNP. Like picric acid, it is often used for derivatizing amines. But you sound
pretty clueless, in all honesty. This stuff is toxic, and is explosive - not a very good explosive but, nonetheless explosive. Those are two good
reasons for it not to be in the hands of someone who needs to be spoonfed about making it, or buying it.
[Edited on 23-12-2007 by Sauron]chloric1 - 22-12-2007 at 17:12
Contacted Chloric about this. This is very odd. Chemoleo
[Edited on 23-12-2007 by chemoleo]MagicJigPipe - 22-12-2007 at 17:20
What the hell? Am I hallucinating?Sauron - 22-12-2007 at 18:11
No, you are not hallucinating, but those should go away as soon as the mods get a look at them. Looks like total gibberish to me.Fleaker - 22-12-2007 at 18:13
He's never done this before, there is very little chance of it actually being him.chemrox - 22-12-2007 at 18:33
Back to ScienceLabs: only work with them on a PO basis so you're not out any cash if they "backorder" you.Sauron - 22-12-2007 at 19:41
I have a better idea: don't deal with ScineLab at ALL. I do not believe they would honor a PO from an individual, and if you have a company or an
institution backing you, then you do not need ScienceLab, do you? You can order from the majors.
Real suppliers usually only honor purchase orders from government entities or institutions. Or established commercial accounts. Getting an account
established is not usually easy.
By buying from ScienceLab you aid and abet known crooks. Maybe not in the legal sense but in the practical sense. They have cheated many of you, don't
help them cheat anyone else.
Where I am, most suppliers will deal with my company on a COD basis. A few ask for payment in advance with first order only. Most will let me order on
a 30 days net basis once I have purchased from them a few times. Now, given one company that gives me terms and another that wants cash in advance or
COD, who do you reckon I will buy from more often? The suppliers know this. They lay ball. Most, anyway.
A few are assholes. The Sigma Aldrich agents are assholes. So is the Cole Parmer agent. The biggest asshole is the PlasLabs agent. He marks up
everything 300% over US retail. So I just buy in USA.
The agents for Acros, Merck, Panreac, Ajax, Carlo Erba, Kimble-Kontes, Fluka (not same agent as Aldrich) are all OK. The Waters HPLC agent is OK.zeppelin69 - 22-12-2007 at 19:57
Quote:
Originally posted by Sauron
This stuff is toxic, and is explosive
[Edited on 23-12-2007 by Sauron]
Thats strange, I was just reading about this compound on Megalomania's site today, and he mentioned its use as a weight loss drug. I can't imagine the
FDA ever approving anything remotely toxic for a daily supplement.
2,4-DNP is an EPA regulated pesticide. It has high acute human toxicity LD50 as low as 14 mg/Kg, and chronic human toxicity as well. EPA has set a RfD
that has a zero in front and quite a few zeros behind the decimal point.
Does that sound like something FDA is going to embrace for tratment of a lifestyle disorder?
Get real.
[Edited on 23-12-2007 by Sauron]zeppelin69 - 22-12-2007 at 20:14
I do not question at all the toxic nature of most nitrophenols, however it apears DNP may be an exception. I may have been wrong assuming that it was
approved by the FDA , but it is still used by many people with rare cases of problems from it. http://en.wikipedia.org/wiki/2,4-Dinitrophenol
Well I have been trying to get the Wiki link to work, but it won't cooperate, sorry.
[Edited on 23-12-2007 by zeppelin69]Sauron - 22-12-2007 at 20:25
Yeah, and on the Internet, hydrazine hydrate is also a recommended treatment for cancer victims. Only problem is, it's a known human carcinogen
itself.
Don't take your pharmacological information from dubious sources, and Wiki is as dubious a source as they get.
From the page I cited above:
Chronic Effects (Noncancer):
* Chronic (long-term) oral exposure to 2,4-dinitrophenol in humans and animals has resulted in the formation of cataracts and skin lesions and has
caused effects on the bone marrow, central nervous system, and cardiovascular system. (2)
* The RfD for 2,4-dinitrophenol is 0.002 mg/kg/d based on cataract formation in humans. (4)
That's two MICROGRAMS/Kg/day.
Having had cataracts, I don't recommend anything that CAUSES them.
If you knew anything about the history of industrial hygiene in explosives factories and munitions plants you would know that nitroaromatics in
general, with no exceptions I am aware of, are highly toxic. That includes nitrobenzenes, nitrotoluenes, nitroanilines, nitrophenols,
nitrochlorobenzenes, nitroxylenes, nitronapthalenes, on down the line. Assuredly some more than others. The ortho-nitro compounds tend to be worst.
Dinitrochlorobenzene is a skin sensitizer, causes severe itching.
[Edited on 23-12-2007 by Sauron]MagicJigPipe - 22-12-2007 at 22:31
Wiki says DNP was used as a dietary supplement in the 30s. I wouldn't doubt this. Remember that back then some considered smoking to be healthy.
I used to work at a local Powerhouse Gym and now that I think about it I remember some of the guys I used to work with (the ones that did the
bodybuilding competitions) mentioning DNP. Also, at that time (about 6 years ago) they talked a lot about how to obtain GHB.
Interestingly, I remember us selling a concentrated ephedra extract which I estimated, at one point, to contain well over 20g of ephedra. I didn't
understand why we stopped selling it then but I managed to grab the last bottle. I still have it today, I guess I should get rid of it.not_important - 22-12-2007 at 22:54
DNP was used as a diet drug pre-WWII, several countries including the US discontinued its use around then. However some people continued and still use
it for its fat burning effects, just as people ingest other banned and/or harmful substances. If you read the Wiki article given it roughly does say
this.
As for hydrazine, while I am rather skeptical of its effectiveness, it should be noted that many drugs used to fight cancer are carcinogenic
themselves; see cyclophosphamide, busulfan, and streptozotocin for examples.Sauron - 22-12-2007 at 23:06
Well, I have good news and bad news for the thread author.
The good news is that per Vodel's 3rd edition, te conversion of 2,4-dinitrochlorobenzene to dinitrophenol does not require an autoclave. His procedure
on a 50 g basis id one in a 1 L RB flask with a reflux condenser and uses sodium carbonate soln and 24 hours reflux. Yield 26 g 2,4-dinitrophenol
after acididying the mixture with hydrochlorice acid.
Now the bad news.
According to Davis, the nitration of chlorobenzene is done with fuming nitric acid (d.1.50) and conc sulfuric acid. The nitration is not difficult,
but for someone who can't buy 2,4-DNP, buying fuming nitric acid may well be just as much of a roadblock.
He could of course make his own fuming nitric acid, by the expedient of KNO3/conc H2SO4 distillation. This has been explicated fully many time on this
forum, with photos, please UTFSE. This procedure is best done either outdoors or in a fume hood, in my opinion, with proper safety equipment at all
times: goggles and gloves at the bare minimum.
So three steps
Make fuming nitric acid
Make 2,4-dinitrochlorobenzene from chlorobenzene
Convert that to dinitrophenol
If the thread author can't buy chlorobenzene, he will have to learn how to chlorinate benzene - not that benzene will be any easier to obtain!
Vogel, Practical Organic Chemistry, 3rd ed. in forum library for download
David, Chemistry of Powder & Explosives, also forum library for download.
See? Knowledge costs nothing.
So, is there any simple way out of this box?
Preparation of trinitrophenol (picric acid) from phenol is possible, by direct nitration with mixed acids, the nitric acid being normal concentrated
d. 1.42. Davis gives this So the problem is stopping at the dinitro stage and then purifying the product to remove any mononitrophenols,
2,6-dinitrophenol, and picric acid byproducts. See what a mess this would be?
[Edited on 23-12-2007 by Sauron]Sauron - 22-12-2007 at 23:13
Some bodybuilders and notably pro jocks also fuck themselves up on steroids in a quest to gain an edge. The results are often personally,
professionally, and medically disastrous.
So fads at the gym do not at all impress me, except to underscore my cynicism about human folly.
Here is what Merck Index 12th ED SAYS ABOUT TOXICITY OF 2,4-dnp
Note: Caution: Highly toxic material. Readily ab sorbed through intact skin. Vapors absorbed through respiratory tract. Produces marked increase in
metabolism and temp, profuse sweating, nausea, vomiting, collapse, death. May cause dermatitis, cataracts, wt loss, granulocytopenia, polyneuropathy,
exfoliative dermatitis, Clinical Toxicology of Commercial Products, R. E. Gosselin et al., Eds. (Williams and Wilkins, Baltimore, 4th ed., 1976)
Section III, pp 134-137.
Sound like a harmless fat burner to anyone???
[Edited on 23-12-2007 by Sauron]MagicJigPipe - 22-12-2007 at 23:32
Agreed. Ironically, a lot of the "health buffs" there were some of the most unhealthy people.not_important - 23-12-2007 at 00:21
hmmm ... nitration of salicylic acid might do. If it didn't decarboxylate during the nitration won't pass the dinitro stage, and it might give a bit
less tar than using phenol. I remember it can be done with "fuming" nitric acid, or standard mixed acid after just plain nitric to get to the
mono-nitro stage. The question is then can the dinitrosalicylic acid be reasonably decarboxylated?Sauron - 23-12-2007 at 00:54
Especially in the hands of a tyro. Given that the dinitro compound is likely to be somewhat explosive, and the most likely decaroxylation technique is
heat...I would be hesitant to go this way.
On the other hand Rosco_B. likes this route to picric acid so maybe he has some thoughts?
I'm sure I made mononitrophenols in teaching lab as an undergrad, I remember the tar and I am sure we only used conc nitric and sulfuric. Going in two
steps and limiting the amount of acid in second step (both steps) ought to give a mix of 2,4 and 2,6- DNPs. Purifification ought not to be too much of
a hassle. ??
Org Syn is not helpful re dinitrophenols or dinitrochlorobenzene.
Vogel has prep of mixed mononitrophenols and seperation of these. Dilute nitric acid.
And he has prep of picric acid from mixed ortho and para pehnolsulphonic acids.
I think I will check PATR and see if they offer any help.
[Edited on 23-12-2007 by Sauron]not_important - 23-12-2007 at 02:06
Well, tri-nitro benzoic acid decarboxylates in boiling water, so there's a chance di-NO2 salicylic acid might do the same with perhaps a boost from
copper salts. But I can't find anything giving examples with that or related compounds so it's just speculation.Sauron - 23-12-2007 at 02:14
The lit. says 2,4-dinitrochlorobenzene can be obtained by nitration of o-nitrochlorobenzene, and that the seperation of the resulting mixture of 2,4
and 2,6 isomers is accomplished by alkaline ethanol-water solution. See Merck Index 12th. entry on 1-chloro-2,4-dinitrobenzene.
Direct nitration of anisole turns out to be hazardous and it is usually prepared through the picryl chloride, itself from 2,4-dinitrochlorobenzene. So
no help here.
Back to the books.
(later) I went out for a dinner and now am back but too bloated to get anything done so will tackle this afresh tomorrow.
Looks like o-nitrochlorobenzene -> 2,4-dinitrochlorobenzene -> 2,4-DNP and a pair of references from Ann. and J.Chem.Soc.
Also Davis talks about a French process from phenol and sulphonation that allows seperation out of the 2,4-DNP (insol in the reaction mix)
So there may be some hope.
[Edited on 23-12-2007 by Sauron]
[Edited on 23-12-2007 by Sauron]
My deepest apologies
chloric1 - 23-12-2007 at 08:56
Hey guys! I am really sorry about those posts. Someone really had a good time at my expense. I will make sure I close this website if I leave my
computer even for a second.
To stay genuine with this topic, the first time I discovered Science Lab I did not like there prices and I did not feel comfortable with there website
at all. I have not purchased any chems from a lab dealer in more than a year. I either have been synthesizing stuff from my stockpile or bought some
chems from pottery suppliers and garden shops. There is enough to keep a working married guy with a child more than busy.Sauron - 23-12-2007 at 21:41
Okay, now I have this nailed.
Start with chlorobenzene.
Nitrate with mixed acid consisting of 30% conc HNO3, 56% conc H2SO4 and 14% water. Temperature 40-70 C. The usual conditions for aromatic nitration
apply, i.e., vigorous stirring and reflux.
This will produce a 95% yield of nitrochlorobenzenes consisting of about 35% 2-nitrochlorobenzene, which is low melting, and 65% 4-nitrochlorobenzene,
much higher melting. These are readily seperated by repeated fractional crystallizations in a procedure described in Ullmann.
Further nitration of the purified 4-nitrochlorobenzene produces only the desired 2,4-dinitrochlorobenzene. This is done at 60 C with mixed acids
consisting of 35% conc nitric acid and 65% conc sulfuric acid.
This contrasts with nitration of 2-nitrochlorobenzene which is said to give 90% of the desired isomer plus 10% of the 2,6-dinitrochlorobenzene.
Fortunately, as the para mononitro isomer predominates, this is not inconvenient.
If you dinitrate the mixture of ortho and para nitrochlorobenzenes, therefore, it would be expected that 10% of the 35% ortho isomer present would be
converted to 2,6-dinitrochlorobenzene.
The French procedure for seperation of the two isomeric dinitrochlorobenzenes could then be applied. This procedure is referenced in the Merck section
above. (Alkaline ethanol-water soln.)
Once pure 2,4-dinitrochlorobenzene is on hand, use the Vogel procedure to convert it yo 2,4-dinitrophenol.
So you have your choice of nitrating pure 4-nitrochlorobenzene, or of using the crude mixed isomers and then removing the 3-4% of the 2,6-isomer from
your 2,4-DNCB.
My advice would be to go the more elegant and seperate the mononitrochloro isomers, then nitrate only the 4-nitrochlorobenzene. You will then have
pure 2,4-isomer and thus, after hydrolysis, pure 2,4-dinitrophenol.
After all the details of the French procedure may be hard to come by, and even if you can get them they will need translation.
This is as simple as it gets. No fuming acid required. No nitration of phenol. You should note that the nitrochlorobenzenes are toxic and you need to
guard against skin contact, inhalation of fumes, etc. Do this outdoors or in a fume hood, wear gloves and goggles, a lab coat, etc.
[
[Edited on 24-12-2007 by Sauron]
Attachment: 24DNCB.txt (3kB) This file has been downloaded 1272 times
Sauron - 24-12-2007 at 02:07
Being concerned that the Ullman definition of mixed acids for nitration was a trifle vague as to concentration of the HNO3, I delved a little deeper.
Unfortunately PATR was not much help.
I found a prep of monochloronitrobenzene in Fundamental Processes of Dye Chemistry (forum library) but it employed fuming nitric acid d.1.52. Likewise
the direct dinitration of chlorobenzene in same volume employed the same fuming nitric acid. Not so convenient for the thread author.
Merck Index 12th ed. references J.Chem.Soc 1006(1948) for prep of mixed isomers of DNCH from nitration of o-nitrochlorobenzene. The acids used in
nitrating mixture are ordinary concentrated reagents, nitric acid d 1.4 and sulfuric acid d.1.84. I will modify this convenient and simple procedure
by replacing the ortho compound with p-nitrochlorobenzene so that we will obtain pure 2,4-dinitrochlorobenzene rather than the isomer mix that the
ortho compound gives.
Dissolve 315 g 1-chloro-4-nitrobenzene in 1300 ml conc sulfuric acid in a 3-neck round bottom 3-Liter flask. Slowly and with stirring add 315 g conc
nitric acid dropwise. After addition reflux the mixture, with continued stirring, on boiling water bath (100 C). Let the mixture cool, then pour onto
2 Kg cracked ice. The product seperates as a yellow oil that will crystallize to a yellow cake. Filter, remelt under water to remove traces of acid,
cool, let solidify, filter again and wash. 2,4-dinitrochlorobenzene is insoluble in water. Once dry, mp 51 C.
So now all we need is a nitration of chlorobenzene to the mononitro products, I believe Vogel gave us that in the form of prep of the
p-nitrobromobenzene, which we can simply used by analogy.using standard acids. Ullmann and Vogel both have direction for seperation of the o- and
p-isomers. This page from Vogel is attached.
As long as the thread author can obtain (or prepare) chlorobenzene, he now has all the information needed to get to 2,4-dinitrophenol without needing
anything exotic.
Which gives a convenient chlorination of benzene, though as sauron noted above, in my case the 2,4-DNCB contained some byproduct 2,6-DNCB (which
doesn't matter if its to be further nitrated, but will matter in your case).Sauron - 24-12-2007 at 03:13
I probably ought to rewrite that Vogel prep specifically for chlorobenzene. Let's scale it up 10x at same time.
In a 3 liter round bottom three-necked flask fitted with a mechanical stirrer, a reflux condenser and a dropping funnel, place 200 ml (285 g) of
concentrated nitric acid. Slowly in a thin stream from the dropping funnel add 200 ml (370 g) conc sulfuric acid. Cool the mixture to room
temperature.
Charge the addition funnel with 102 ml (113 g) of chlorobenzene. Add this dropwise with vigorous stirring to the mixed acids, not allowing the
temperature to rise above 50-60 C. Once the addition is complete and exothermic reaction has subsided (no more rise in temperature), heat the reaction
mixture on a boiling water bath for 1 hr. Continue the mechanical stirring throughout the heating period.
Remove from bath, discontinue stirring and allow to cool to ambient.
Pour into 2 Kg cracked ice. If the nitrochlorobenzene does not immediately srystallize, stir until the oil solidifies. Filter, wash with water, and
drain as well as possible. Recrystallize from 1 to 1.2 L 95% ethanol heated on a water bath to just under boiling (75-78 C). Let cool. Filter the
precipitated p-nitrochlorobenzene. The mother liquor contains the ortho isomer contaminated with some p-isomer.
Yield about half a mol of pure p-isomer. (70-75 g)
-----------------
Thanks, Axt. If the thread author can't get benzene or chlorobenzene, he still might have a better chance of getting sodium benzoate, and TCCA
(swimming pool chemical) ought to be a snap. That's a very nice series of preps you have there. I had not looked at them before.
[Edited on 24-12-2007 by Sauron]Ozone - 24-12-2007 at 06:21
Sauron is not kidding!
Some brief notes on the toxicity of dinitrophenols:
1. Look up electron transport, then imagine it running out of control (then imagine uncontrolled anorexia). Nitrophenols have a tendency to eliminate
via urine and have been demonstrated to increase the risk of bladder cancer.
2. From elsewhere on this site (quoting myself):
"...sec-butyl-2,4-dinitrophenol (Used at the time as a polymerization inhibitor) goes straight through nitrile gloves. I developed a migraine, fast
irregular heartbeat, I was *hot*, sweating profusely. I removed my gloves to find that I had yellow fingers. Not good. I went outside, (it was cold,
thank goodness) sat down and had a smoke (tasted like DNP and metal). Fortunately, this went away, but the dose was small and *transdermal*. yikes..."
Remember that your intermediate products are toxic as well!
Take care and merry Christmas,
O3Sauron - 24-12-2007 at 19:06
Damned right they are toxic. 2,4-DNCB is not an obscure compound, it has been mass manufactured for a very long time because of its vast strategic
importance in the explosives and even moreso, the dyestuffs industries. So its toxicity has been amply documented and well studied. It is a notorious
itching powder, producing eczema and unbearable itching upon contact with the skin, especially when in solution. The French actually used it as an
explosives additive in shells (or left it in as an impurity) precisely because they liked this harassing effect on enemy troops.
Incidentally, pure 2,4-DNCB is regarded as somewhat less toxic than mixtures of 2,4- and 2,6-DNCB which implies that 2,6 isomer is far more toxic than
the other. As mentioned, the ortho to para ratio for mononitrochlorobenzene is about 33/66 with balance traces of m-isomer. And further nitration
produces c.97% 2,4-DNCB and 3% 2,6-DNCB because all of the p-isomer gives only the 2,4-isomer while the o-NCB gives 90% 2,4 and 10% 2,6. So 10% of 33%
is 3.3%.Alan - 25-12-2007 at 08:22
I would not recommend buying ANY thing from there. I know way to many people that got dicked around for a couple MONTHS or they NEVER even received
what they sent money for.
Originally posted by chloric1
.....the first time I discovered Science Lab I did not like there prices and I did not feel comfortable with there website at all. I have not
purchased any chems from a lab dealer in more than a year.....
I'm not in the habit of bashing a company but that one really gets me going. I placed a rather large order with them which was not delivered, etc,
etc. They charged my card, bla, bla. They gave me the run-a-round like I have not had in quite awhile ...They are extremely haphazard in their
business practices. Never again.
