I've always been fascinated by dyes and indicators, and have been wanting to try synthesizing a little fluorescein for a long time. I already have
some disodium fluorescein, but it seems like it would be a very interesting synthesis to try out--maybe by Woelen's method.
My question is this: <strong>Would it be illegal (Minnesota, USA) or even questionable to purchase 500 grams of phthalic
anhydride</strong> for this purpose? I've always been wary of purchasing <em>any</em> organic compound, because of concerns over
legality--I only have a few organics, and they're practically useless, like 500 g of lab grade 1-hexadecanol flake.
I've done hours of Google and forum searching, and have been unable to find anything on this. Am I just inept at searching? Where could I find more
information about what compounds are on precursor/controlled substances/whatever lists in my area?
(I'd rather buy less than 500 g, say about 10-30, but the only quantity available on eBay is 500 g.)
Again, I'd like to apologize if this has been answered elsewhere. If necessary, please delete this thread. Thanks.
[edit]
Rephrased my question.
[Edited on 3/15/08 by bfesser]MagicJigPipe - 15-3-2008 at 08:05
Although your paranoia is well founded, I don't think phthalic anhydride is a big deal. I know it's not listed and I can't think of any common drug
syntheses that it is used in. It can be used in a round about way to produce thionyl chloride which is considered a chemical weapons precursor but
the synth is so convoluted that I doubt you will find any resistence.
There are several places on this forum where list 1 and 2 chemicals (US) are posted. Or you could just try searching google for list 1 and/or 2
precursors. I don't want to post them again here because, like I said, they're all over the place.
Another thing, you won't get very far in home chemistry without using any organics. I mean, ethanol and rubbing alcohol (isopropanol) are organic
substances and you certainly don't have to worry about those.bfesser - 15-3-2008 at 08:19
I didn't take ethanol, isopropanol, or other ubiquitous organics into consideration when I made the statement 'few organics', but you are very right
that one can't get far without organics. Thank you for your help, it's greatly appreciated.smuv - 3-4-2008 at 13:36
It could be used to make phthalimide which can be used to make methaqualone (quaaludes) via a few different routes. Although I wouldn't worry about
it.
Phthalic acid can be produced via oxidation of naphthalene (in either gas or liquid phase). Additionally xylene could be oxidized to mixed phthalic
acids, it may not be too hard to separate these acids as only one isomer would dehydrate to the anhydride upon sublimation.pantone159 - 3-4-2008 at 14:17
I would not be concerned about pthallic anhydride.
(Note: The SM spell-checker wanted me to change 'pthallic' to 'phallic' )Sauron - 3-4-2008 at 14:23
O-xylene can be purchased pure. Mixed xylenes are cheaper but you pay one way, or you pay another way, as with all things.
Phthalimide in not listed and not watched. Anthranilic acid, which can be made from phthalimide as well as other ways, is, or was. (The other required
component for methaqualone being o-toluidine.)
However since ludes ceased to be a problem, I am not at all sure anyone really cares anymore, they have other fish to fry.
And I hate to tell you, pantone, but there are two h's and only one l in phthalic
[Edited on 4-4-2008 by Sauron]pantone159 - 3-4-2008 at 17:09
Quote:
Originally posted by Sauron
And I hate to tell you, pantone, but there are two h's and only one l in phthalic
Oops. Hard to make fun of the spell checker now.
BTW - anthranilic acid would be very watched, it is DEA List I.smuv - 3-4-2008 at 17:38
I agree with you Sauron, my post was in response to MJP saying that phthalic anhydride can't be used to make any common drug.
[Edited on 3-4-2008 by smuv]MagicJigPipe - 3-4-2008 at 18:56
"I agree with you Sauron, my post was in response to MJP saying that phthalic anhydride can't be used to make any common drug."
Are quaaludes common now?Sauron - 3-4-2008 at 19:13
But, pantone, the spellchecker apparently does not know how to spell phthalic, either.
It is trying for phallic - clearly has its mind in the gutter.MagicJigPipe - 3-4-2008 at 19:29
"It is trying for phallic - clearly has its mind in the gutter."
Oh my god! Hahaha!
Also, is phthalic acid used in any consumer products (not esters)?Sauron - 3-4-2008 at 21:01
Phthalic acid itself is not often encountered, phthalic anhydride is ubiquitous. A major intermediate in many industries.
AFAIK onl the esters are commonly enountered in consumer products, but consult Ullmann's and Kirk-Othmer for more information.smuv - 3-4-2008 at 21:34
Quote:
Are quaaludes common now?
I knew that would be your response. Your are right, outside of africa quaaludes are rare these days. However, since the original poster seems
paranoid about this, I think he ought to know. I'm not saying phthalic anhydride is suspicous but in order to properly inform the poster I think it
is worth mentioning.Sauron - 3-4-2008 at 22:42
As Bill Rotsler used to say:
"Just because you are pArAnOiD, does not mean they aren't out to get you"
[Edited on 4-4-2008 by Sauron]12AX7 - 4-4-2008 at 12:30
1-nitrosyl-4-iodo-deuterobenzene
Para-NO-I-D
Timpyrochem - 2-9-2008 at 21:30
The esters of anthranilic acid are also DEA list 1, but methyl anthranilate aqueous solution (~26%, IIRC) can be purchased in garden stores as bird
repellent. Expensive, but grapey!celindgren - 12-1-2009 at 00:05
Hi,
I would appreciate it very much if someone could assist me in finding Phthalic acid (benzene-1,2-dicarboxylic acid) in small containers which cost
about $50-75. As I need it only for specific endeavours, I do not need very much. At present, the cheapest I can find is over $400.
Dr. Carl Edwin Lindgren, F.R.S.H. JohnWW - 12-1-2009 at 00:34
That is clearly grossly exorbitant, because the ester dimethyl phthalate (DIMP) is a widely made and cheap industrial chemical, used particularly as a
mosquito repellant. I wonder if you could buy some of that cheaply, and hydrolyze it.benzylchloride1 - 7-2-2009 at 14:23
Alfa Aesar lists 1 Kg of phthalic anhydride for around $12.00. I bought some off of Ebay, but it was mainly phthalic anhydride. I ran a synthesis of
o-benzoylbenzoic acid and got a yield of only 45%. The phthalic "anhydride" had a large melting point range and finally melted at about the
temperature that phthalic acid melts at. I decided to purify it by distilling off the water and then distilling the anhydride. The distillation went
well and I ended up with some nicely crystalline material with a very pungent odor. I was using a new short path distillation set up and when I tried
to remove the distillation set up from the plastic clamps that held the apparatus together, I heard a cracking sound and there was a large jagged hole
in the glass. The plastic clamp had melted to the glass and when I removed the apparatus, I broke my distillation set up. Next week I will have to fix
it at the university. When I tried to remove the anhydride from the receiving flask by chipping the material out, I ended up cracking the flask.
Beware of non anhydrous phthalic anhydride!S.C. Wack - 7-2-2009 at 15:23
This is not on any DEA list in the USA. It can be made from mothballs (see Cumming here or at 4shared), but as written requires nearly an equal weight
of HgSO4, and quite a lot of H2SO4.Magpie - 14-6-2010 at 13:20
I have purchased purported phthalic anhydride from two different sellers. In both cases the melting point (191C) indicated I had phthalic acid
instead (phthalic anhydride mp =131.5C). I'm feeling quite ripped off and plan on calling these suppliers to complain and seek replacement or a
refund.
I sublimed a small amount of the white flake sent from the first supplier into fine needles of phthalic anhydride which indeed had a mp of 131.5C. I
would just shut up and sublime what I need except it is like collecting cobwebs and may take a lot of effort to collect just a few grams.
Has anyone else other than BZ1 had this problem? Any recommendations? MagicJigPipe - 20-6-2010 at 13:43
What was the melting range, Magpie?Magpie - 20-6-2010 at 16:32
There was a range for both suppliers' products but I didn't necessarily record it.
The mp I recorded for the 1st supplier is 194C.
For the 2nd supplier, I ran 3 mp's:
*powder sample from top of bottle: >140C (quit raising temp)
*crushed flake from deep in the bottle: partial melting & slumping at 131-132C
*crushed flake from deep in bottle: no slumping, mp = 190C. Magpie - 1-7-2010 at 12:10
I have received yet another bottle of phthalic anhydride. But its melting point is also 191C, indicating it is really phthalic acid. That's three
different lots now all testing false.
I'm beginning to wonder if it is something I'm doing wrong. If possible I would like to hear from other members who have phthalic anhydride. What
melting point do you get? Magpie - 4-7-2010 at 16:33
Having given up on being able to get phthalic anhydride (PAN) from suppliers (they send me phthalic acid [PA] instead), I have developed a reasonably
facile procedure for converting PA to PAN:
In a hood or outside:
Place 25g of the PA in a 250 mL beaker supported by an iron ring attached to a ringstand. Place the beaker in an oil bath so that the PA is heated by
the oil. Set the bath temperature at 200C. As the PA is heated above its mp (191C) PAN and water will vaporize. Some of the PAN will be lost to the
atmosphere and some will accumulate as fine needles in a wool along the sides of the beaker. Gather the wool as it is generated and drop it back into
the melt. Continue this until the melt has turned from milky white to clear. Then pour the melt into an evaporating dish and place in a dessicator
to cool. When cooled scrape out the melt and grind to a powder with a mortar and pestle. Yield = 82%.
I have done this twice. Both times the mp of the resulting PAN was 131.5-132.0C, as it should be.
DJF90 - 5-7-2010 at 07:29
Very nice work Magpie! Good that the melting point is correct also.entropy51 - 5-7-2010 at 08:38
Very nice indeed, Magpie! quicksilver - 5-7-2010 at 09:18
In the start of this thread a gentleman asked if some material was restricted or "illegal" & the logical response made that material didn't exist
on List 1 or List 2 chemicals. However there are more than the DEA List 1 & 2.
There is a DHS "List of Watched Materials" which I once tried to post but the damn thing was over 2Mb (compressed even as text!) so I couldn't put it
up. In this discussion another individual made the remark that the material in question didn't appear to be a precursor to a chem-wep, etc. And there
is where the issues become complex. The DHS list includes some esoteric materials that many would not consider as being significant yet are so in lab
or plant-level production of items that are far from common.
The DHS list does not appear to have threshold amounts. In some materials the level of toxic utility is high enough that such a thing is immaterial.
The DEA realized this when dealing with micro-gram level dose applications and changes were made. DHS never approached their agenda with
threshold-levels in mind.
Because of their annoyingly secretive agenda; INTERPOL may have a list of watched materials (it may be where the DHS list was drawn from). However I
was unable to find international organizational restrictions on chemicals or apparatus other than United Nations agreements, etc....
However, the level of discussion is out there & bold!
(cut)
Because of their annoyingly secretive agenda; INTERPOL may have a list of watched materials (it may be where the DHS list was drawn from). However I
was unable to find international organizational restrictions on chemicals or apparatus other than United Nations agreements, etc....
Many of the international arrest warrants indiscriminately issued by Interpol, on request from various governments, are for what amount to alleged
purely political offenses. In New Zealand, there is a political refugee from Algeria, Ahmed Zaoui, who was jailed for several years before being
released and given asylum, because of a false arrest warrant delivered by Interpol on request from the Algerian Government, a dictatorship which
alleged that he was wanted on criminal charges that turned out to be false and politically inspired.
This sort of thing is a good reason for national Constitutions or Bills Of Rights to be amended to prevent a country's own nationals from being
extradited for any reason for alleged offenses committed in foreign countries, because of the danger that such allegations of offenses could be
politically-inspired. This is already the case with France, Russia, most other eastern European countries, most Latin American countries, and several
Asian countries including China and Vietnam. But this is, unfortunately, not the case with the UK, where the alleged "UFO hacker" Gary MacKinnon is
still in grave danger of extradition to the U$A, a country he has never visited, for allegedly hacking NASA's website, based on a server in Virginia,
to hunt for suppressed UFO-related information.
In the case of the U$A, the DOJ takes it upon itself to arrest and try U$ citizens for alleged offenses committed in foreign countries, which because
of the difficulty of getting witnesses and material evidence out of foreign countries for use in U$ Courts (it would be impossible for a foreign Court
to be induced to make such orders except for war crimes trials) could result in huge miscarriages of justice. If accused U$ citizens are also tried
and jailed in the foreign countries in which they are alleged to have committed offenses, double jeopardy could result on deportation back to the U$A
after serving jail sentences overseas.
[Edited on 6-7-10 by JohnWW]Gruson - 21-7-2010 at 06:26
I just ran a melting point test on my hotbench, and the phtalic anhydride provided by Jor has a melting point of 193 degrees centigrade. So it is also
phtalic acid. Pretty needles though when it melts and partly vaporizes.Magpie - 21-7-2010 at 07:34
I just ran a melting point test on my hotbench, and the phtalic anhydride provided by Jor has a melting point of 193 degrees centigrade. So it is also
phtalic acid. Pretty needles though when it melts and partly vaporizes.
Hello Gruson! So you are the 3rd person now reporting that their purported phthalic anhydride is actually phthalic acid. So what gives with this. I
didn't find my phthalic anhydride to be particularly hygroscopic.
Phthalic anhydride is supposed to be so much cheaper than phthalic acid. You would think it wouldn't be so hard to find.
)
