Author Topic: For the vindication of Eleusis - Methylamine  (Read 56863 times)

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armageddon

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-
« Reply #100 on: July 23, 2004, 01:26:00 PM »

moo

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Moderators?
« Reply #101 on: July 23, 2004, 04:38:00 PM »
Back at it again, huh? Where the heck are the moderators? It's obvious that the dicksizing is getting harmful to the Hive collective. Take it to the couch or PM if you really have to, this place is for discussing chemistry. Neither one of you is going to "win the argument with the other one", it is futile. Why's that? Because it appears neither one of you is going to admit the other one was right nor are you going to reach an agreement/compromise/synthesis because all that seems to matter is "I was right, thus he's an asshole". Is that so important?


Bond_DoubleBond

  • Guest
armageddon: swim recrystallizes with methanol...
« Reply #102 on: July 24, 2004, 04:47:00 AM »
armageddon:

swim recrystallizes with methanol and knows how to separate amcl from meam.  watch who's yields you call bullshit.

edit: sorry, i though you were talking to me.

armageddon

  • Guest
repeating my guess
« Reply #103 on: July 24, 2004, 06:57:00 AM »
BDB: I surely don't question your skills, and believe honestly you belong to the bees having mastered the patented procedure very well. Sorry if you got any other impression - was just a bit upset, actually I was referring to Abolt's claimed 93% yield..
(in fact your yields are quite good I think!)

And to repeat something hidden in one of my downrated posts, but which I still consider being of importance - here we go:

here's my thoughts on why the patent uses additional alcohol:

I think the reason for using ethanol is to remove excess formic acid (the formic would otherwise methylate the MeAm further to diMeAm) resulting from too much formaldehyde. This means the reaction evolves no CO2 and doesn't stink from formaldehyde escaping the apparatus.

And this process of "removing" the formic by reacting it with ethanol is easily controllable by adjusting the distillation of formed ethylformate - because a reaction from which one (or more) products (and NOT educts like alcohol) are contiuously removed DEFINATELY proceeds faster, according to LeChatelier (or why else should dean-stark traps work for Knoevenagel rxn for example??).

And as the difference between the boiling points of ethylformate and ethanol is less than 30°C, it is necessary to distill carefully (either by using some column or by distilling slowly) in order to properly separate the formed ethylformate WITHOUT distilling the unreacted ethanol together with it.

If these two aren't separated properly and/or distilled away too quickly (i.e. before all formaldehyde has reacted), their use is obsolete, as the removal of excess formic is not possible anymore - it simply decomposes, and part of it causes polymethylamine formation.



I honestly believe (and can come up with explanations for every of my statements, if anyone desires so) that this is the reason for using alcohol, and the advantages arising from using it justify well why the IG-Farben company got the patent granted back then..





And to complete my suggestion about the possible benefits of the patent, here is a precise translation of some "key sentences", translation more accurate than the one provided by Orgy (no flame Org;  but I spent ALMOST an hour to retranslate these few sentences as EXACTLY as possible because I believe they are vital to understanding for non-german-speaking bees, and I doubt you did so when discovering/testing/posting the whole lot back then..  ;) )

"Besides of avoiding the oxidation of formaldehyde to carboxylic acid, the use of additional alcohol also has the advantage of allowing the reaction to proceed at 75°C, whereas without alcohol the reaction only sets in at >90°C.
Other advantages being the reaction speed is increased considerably and the tendency for forming higher methylated amine gets significantly reduced.
"

It might be helpful to keep this in mind before speculating further about the topic, so here you can reread about what advantages this patented procedure should offer if done correctly.

(BTW: WOW! Now that's what I call a "rating session"! Thanks.)

Greetz A


abolt

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(Post deleted by abolt)
« Reply #104 on: July 26, 2004, 05:32:00 AM »
(empty)


Organikum

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obsolete now
« Reply #105 on: July 26, 2004, 05:57:00 AM »
obsolete after Abolt deleted his post.

LaBTop

  • Guest
Now youz' all BEEhave again,
« Reply #106 on: July 26, 2004, 02:36:00 PM »
after reading this carefully:
 
--------------------------------------------------------------------------------
Not long ago I expressed the view that the lack of general education and of thorough training in chemistry of quite a few professors of chemistry was one of the causes of the deterioration of chemical research in Germany. Will anyone to whom my worries seem exaggerated please read, if he can, a recent memoir by a Herr van’t Hoff on ‘The Arrangements of Atoms in Space’, a document crammed to the hilt with the outpourings of a childish fantasy. This Dr J H van’t Hoff, employed by the Veterinary College of Utrecht, has, so it seems, no taste for accurate chemical research. He finds it more convenient to mount his Pegasus (evidently taken from the stables of the Veterinary College) and to announce how, on his daring flight to Mount Parnassus, he saw the atoms arranged in space.

Hermann Kolbe (1877).

This lacerating type of criticism was not uncommon in the 18th and 19th centuries. G.S.Ohm was rendered incapable of working as a result of the vitriol heaped on his work which led to Ohm’s Law. Kolbe was no chemical slouch; he was one of the foremost chemists of his day. Unfortunately he was dead by 1900, when J H van’t Hoff received the first Nobel Prize in chemistry – for his work on the shapes of molecules!
--------------------------------------------------------------------------------

All of you _could_ be one day famous underground chemists.
Don't lactate your future reputation with so much unnescessairy venom in our chemistry forums.
LT/


bbeeasheets

  • Guest
my first meam.hcl synth
« Reply #107 on: July 29, 2004, 09:28:00 PM »
Here is what I did.

100g pulverized hexamine.
30g nh4cl

put in 1L RBF
added 130 mls denatured ethanol (distilled to 95%)
added 330g muratic acid (beaker on scale, tared, poured hcl to 330g..? not sure if this is the way to calculate this. I tried to calculate by weight of hcl, but volume was 968 mls or something, so volume was to great.

Here is where i noticed my first problem, the powder did not completely disolve no matter how much stirring i did.

Gradual heat applied to distilling app.
(since I have never used this plate before it took almost 6 hours to reach 60C and distill the formates.

at this point i turned up heat and bolied until it reached 100C

I then cooled to room temp and vacuum filtered the solids, then returned them to clean RBF to distill out water

vacuum applied not very strong, h20 boiled over at 90C
I boiled until the crystals around the edges started to look a little crispy.

I then put in 200mls of boiling ipa.
This point my second problem showed up. Very little of the solids dissolved, but i filtered anyway. let cool to rt and stuck in freezer over nite.

the remaining undisolved solids i washed once more with boiling ipa and then added 200 mls of dh2o. The solids all dissolved immediatly. this can't be nh4cl can it?

so i redistilled the water out of the batch of crystals that were redissolved in water. is it worth going any farther with these crystals?

the small batch of cystals that were formed in the 1st ipa wash were filtered and then washed with hot methanol (anhydrous). However I wonder if I used to much methanol, because  they won't recrytallize even at -15C

thanks for any help. yes I am a newbie and I expect flames if you must... hopefully they will help me with my lab technique.

Organikum

  • Guest
You should give the methylamine.HCl some time...
« Reply #108 on: July 29, 2004, 11:13:00 PM »
You should give the methylamine.HCl some time to dissolve in the IPA - that doesnt happen so fast. Give time and stirr whilst keeping it hot.

Why does everybody expect this going in seconds? Even tablesalt also takes quite some time to dissolve in water.

This is no "washing" but extracting with IPA. Whats not in the IPA is ammoniumchloride.

The ways how to do this for best results was extensivly discussed and described in this thread. Read it up, you didnt use the best way, this may be disclosed here and now.


armageddon

  • Guest
big error!!
« Reply #109 on: July 30, 2004, 08:03:00 AM »
bbeeasheets:

The problem of your low yield might lie in your bad extraction technique (better REFLUX in IPA several times than to wash with it!) - but there is a much bigger error in your synthesis, may I quote:

at this point i turned up heat and bolied until it reached 100C

I then cooled to room temp and vacuum filtered the solids, then returned them to clean RBF to distill out water.


...but...

You dont are to collect the SOLIDS gotten after cooling the rxn mixture/before commencing with distillation, these are NH4Cl and should be discarded or better saved for reuse in next batch, IN NO WAY PUT IN A CLEAN RBF AND HEATED!!!! Instead, keep the liquid you separated from the solids, put THIS in clean RBF and reduce its volum by distillation, until no more water comes over or 150°C are reached. hen cool to room temp, and THEN extract the formed, almost-dry, crystalline mass by refluxing it in isopropyl alcohol, reapeating several times with fresh IPA, combining the extracts, concentrating them and then cooling the concetrated solution in the fridge to precipitate methylamine hydrochloride. ALL SOLIDS COLLECTED BEFORE THE IPA XTRACTION ARE MAINLY AMMONIUM CHLORIDE!!


(BTW Organikum: IPA/HCl is indeed smarter!  :) )

[EDIT]OK, the post was "un-shouted"..[/EDIT]

A


armageddon

  • Guest
oh well
« Reply #110 on: July 30, 2004, 08:35:00 AM »
Bbeeasheets: your problem is that you collected the solids and heated them to dry'em - COMPLETELY wrong! You should've separated solids from liquid after cooling to room temp., but kept the LIQUID! This you should've distilled with heating to max. 150°C and then cooled to precipitate ammonium chloride salts, which you then could've xtracted by boiling in IPA...

next time, hm?

[EDIT] Obsolete after my previous post is visible again  :)  [/EDIT]




Huh!? Are you moderating or adjudicating??

To the moderator whoever you are at the moment: could u please un-rate this post?? Not that I care for bad karma, have enuff good to compensate - but I consider the information helpful for Bbeeasheets, as he really made a big mistake. I just edited the text into "sub" markup,

And hey!
   WHY is My PoSt RaTeD aS "aLl CaPs"????? in fact they aren't all capitals, only the relevant part was "capitalized"..

Or is my written presence in this thread not desired?? I mean, NO PROBLEM! I at least AM capable of synthin MeAm, and do understand the talked about patent quite well - if u have the opinion that I should keep my knowledge to myself instead of helping bees with no xperience w/this patent - just go ahead to tell me.

A


Rhodium

  • Guest
You aren't supposed to write in ALL CAPS ...
« Reply #111 on: July 30, 2004, 09:53:00 AM »
WHY is My PoSt RaTeD aS "aLl CaPs"????? in fact they aren't all capitals, only the relevant part was "capitalized"..

Thus the "relevant part" will be the most hard to read section of your post...

You aren't supposed to write in ALL CAPS because it is very hard to read as well as being "shouty" writing.
I have unrated your post, but please uncapitalize that paragraph and use bold markup for emphasis instead.


bbeeasheets

  • Guest
first time errors
« Reply #112 on: August 01, 2004, 06:28:00 PM »
thanks for not flaming me on my stupid mistake(s). Thought I had read everything in this thread well. Anyways maybe I can get as better yeild if it is done right.

Just a few more questions before my next attempt (these are newbie questions, should they be posted in newbie forum?)

alcohol and hcl are stated in grams. does the weight include the water (just weigh an appropiate volume on scale?) or should i calculate the weight by percentage?

thanks

armageddon

  • Guest
measuring volume/weight of liquids...
« Reply #113 on: August 01, 2004, 09:05:00 PM »
alcohol and hcl are stated in grams. does the weight include the water (just weigh an appropiate volume on scale?) or should i calculate the weight by percentage?

As far as I know, the weight is stated for a certain concentration, i.e. 220grams of 31,45% HCl...
(read the first few posts again maybe? I'm sure the concentration is mentioned...  ;) )

So if you use other concentrations of acid and/or alcohol, you should of course calculate for the missing percent - weigh your diluted reagents, but use more... (the extra water won't hurt)

Or if you know the density of certain concentrations of HCl/EtOH, you could as well use a certain volume of each  - probably the easiest way, a slight excess of acid/alcohol is in fact desirable.

Oh, and while we're at it:

Alcohol extraction/recrystalizing of the crude product is ABSOLUTELY necessary to assure you don't have a healthy amount of ammonium chloride in your final product. When the extraction is done properly, ALL remaining solids are pure NH4Cl, and EVERY F****N crystal crashing out of the extract upon cooling is PURE methylamine hydrochloride CH3NH3Cl! 

- just in case you like a clean product of course... ;D

(no offense, but while "mixed amine salts" undoubtedly may be of advantage sometimes (Al/Hg on MDP2P - dont attempt it of course, it's pretty illegal - as the product is MDA/MDMA mixture..), in other cases purity is desired/essential and a NH4Cl/CH3NH3Cl mixture of whatever percentage just isn't suited very well for certain applications... ;) )

BTW thx for unratin me post.. ;)
Greetz A


armageddon

  • Guest
another variation
« Reply #114 on: August 03, 2004, 12:32:00 AM »
Hi!

Based on my reflections about the *real* advantage of adding ethanol to a hexamine/NH4Cl/HCl methylamine leuckart (in fact its a leuckart with formaldehyde!), I just decided to give the procedure outlined in

Patent DE468895

another try, and tried to modify the rxn parameters to challenge the following statements:

    
- According to the patent, one of the benefits would be that the reaction already succeeds at below 75°C, whereas normally >90°C are required.

- Also (and maybe far more important), the formaldehyde, upon oxidation, does result in formic acid - and this formic could normally serve as a methylating reducing agent for MeAm, resulting in diMeAm formation. But with ethanol being present, the acid should ideally be completely converted to its ester (ethylformate), and through removal by distillation, all formed formic acid should (ideally) be removed as it is formed.



These two main statements in the original text can be well taken to the test: by quickly heating the reaction exactly to the point at which ethylformate begins to come over (based on previous runs, I know this point is 85°C on my variac/heating mantle), then holding it there for a long time to make sure all formaldehyde has reacted, all formic was esterified and all formed ethylformate has been removed by distillation (i.e. let it run overnight).

If the above claimed benefits are correct, the reaction should be finished at this stage, as the temperature was held above 75° for many hours and in theory, all "harmful" formic acid should've been removed completely, i.e. from 48g hexamine, one should get 2.05mol of HCHO which in turn can act on 1.63 mol NH4Cl - therefore, ~131ml ethylformate should be formed in theory...

(..and this is well in accordance with the following observation: even far below 80°C, formaldehyde obviously reacts readily with "something" to produce formic which in turn esterifies to EtCOOH - at least there is ethylformate formed long before this temp. is reached! In fact, the threshold for its formation to occur was observed being ~43°C rxn temp...)

And as there are excess ethanol and NH4Cl present, the reaction should ideally give almost quantitative yields (calculated from formaldehyde) of pure methylamine hydrochloride (and the remaining excess of NH4Cl of course) without any di- or even trimethylamine impurities... theoretically at least, or so to say, if the inventors knew what they got patented back then...

So far the theory.




As already said, I wanted to challenge this. The following procedure was used:

48g hexamine (fuel tabs) were dissolved in 100ml warm tap water and filtered through a pad of celite with the aid of vacuum in order to remove any waxes and binders. The resulting clear solution was put in a 500ml two-neck RBF along with a big ass stirbar. Then were added 14g NH4Cl, followed by 90ml EtOH. The RBF was fitted with a distillation rig and 160ml 31% HCl were added through the side neck which afterwards was equipped with a (second) thermometer submerged into the rxn liquid for measuring the rxn temp. HCl addition caused a bit of white smoke to travel down the condenser and the exothermic hex hydrolysis caused the rxn temp to climb to 40°C and everything became slightly milky.

Using a heating mantle equipped w/variac, the rxn was then brought to 80°C (internal rxn temp.) over the course of exactly 1 hour, causing the formation of a clear ethylformate top layer and, upon reaching the said temp., a slight reflux. At this point, the cloudiness had disappeared completely (waterlike, clean).

When the variac controller setting was raised to >80°C (82.5° internal rxn temp.), the ethylformate slowly started to distill with a steam temp. of 42-58°C (I didn't allow it to climb higher but cooled it if it happened; as the proper separation of ethanol and formate isn't warranted anymore if this happens).

The upper layer disappeared quickly within one hour, but formate still came over at a rate of 1 drop every 5-6 seconds while steam temp levelled of at 53°C (rxn. temp. 80.5° C). This is now heated at 85°C overnight...



I'll get back with the results tomorrow!


(just in case...: anyone impeaching above procedure before results are in is immediately catalogued on my "personal asshole N°1"-list as one of the top ranks forever... So control your temper until you can fully judge about it please!!)




[EDIT] exactly 9 hours and 20 minutes of careful heating have passed since I combined the reagents, the internal rxn temp. is still 85°C with ethylformate coming over at a steam temp. of 49°C at a rate of 1 drop every 10 seconds - and interestingly, the solution has become slightly greenish tinted, although the amount of distillate collected is only about 60ml... Just cranked the variac up to 90°C - think I'll let it run for a few more hours.

I'll be back soon...

BTW did you realize the similarities to a leuckart? Slow heating over long time, resulting in faint bubbling due to *slow* decomposition of the reducing agent (only that it decomposes just to formic rather than complete decomposition to CO2 - like would be the case with *real* leuckart - but faint bubbling can be seen in both cases....) [/EDIT]

Greetz A


armageddon

  • Guest
another variation - part II
« Reply #115 on: August 04, 2004, 02:14:00 AM »
After 11 hours of heating (with raising the temperature of my heating mantle to 150°C during the last 2 hours), the rxn temp was 112°C, with steam temp being 100°C - and then I broke the long thermometer - aaargh! (no more rxn temp. measurements  :( )

Anyway: the solution was concentrated to 2/3 of its original volume and turned to a yellow color while no formaldehyde smell could be detected anymore.
 
It was cooled to 7°C, vac filtered and the crystalline mass extracted by boiling in 100ml IPA for 10 minutes (just to be sure), then the crystals were washed sparingly with cold IPA and dry acetone and upon drying became crunchy and bone-dry (i.e. only NH4Cl, as CH3NH3Cl is pretty hygroscopic).

The mother liquor and washings were combined with the IPA extract and concentrated to about 180ml (variac set to 155°C) and poured into a beaker while still hot (HCl fumes evolved),  cooled in the fridge, vac filtered (this time the precipitate had quite a bit of MeAm in it, judging from the many little plate-shaped crystals) and the precipitate again extracted with boiling IPA (2x with 80ml this time). The combined extractions, washings and mother liquor (deep yellow now!) were then again freed from solvent through vacuum distillation (variac still set to 155°C, pretty quick dist.!). As the volume of the remaining liquid reached ~150ml, *lots* of little shiny platelets appeared in it, while a small amount of white "smoke" appeared inside the condenser - probably HCl(g), as it dissolved in the distilled IPA before having passed half way down the condenser...

As soon as the IPA had been removed completely, the crystals floating in the solution redissolved completely (higher solubility of MeAM*HCl in water than in IPA). Concentration was continued (variac setting 200°C) until signs of crystal formation again became visible on the side walls, then the hot solution (which had changed colour to deep orange) was poured into a beaker(crystallized immediately), the flask rinsed with boiling IPA, and everything (concentrated soln. and IPA rinse) was slowly cooled to -7°C.

the result was one hard lump of orange crystals which were vac filtered, rinsed with a bit ice-cold IPA followed by acetone, sucked dry by pulling air through them for ~5 minutes and placed in a clean, dry 500ml 2-neck RBF. To this was added 150ml IPA and everything was refluxed for 30 minutes, then (after the boiling had just subsided) the IPA extract was carefully poured off into a big erlenmeyer, and the process was repeated 4x with fresh IPA. The remainder was isolated by vac filtration and rinsed with boiling IPA followed by acetone, the combined IPA extracts and washes were then concentrated, resulting in a small amount of NH4Cl precipitating on the flask walls, and the IPA solution became clear again. Upon further concentrating, much MeAm*HCl crystallized ( hexagonal shiny plates). The still hot IPA soln. was then poured into a beaker and cooled to -7°C.

The decanted solution solidified to a slightly orange-tinted, crystalline mass consisting of  *lots* of tiny little plates. The crystals were vacuum filtered, washed sparingly with cold acetone and the mother liquor again concentrated and crashed out with dry acetone. The (still moist) crystalline MeAm*HCl was then slurried with some water, put in a 2-neck RBF and conc. NaOH solution dripped onto it - the resulting methylamine gas was taken up in ice-cold MeOH which was weighed before and after gassing, to determine the amount of MeAm(g) taken up.

(...)






The theory behind the workup is that the NH4Cl precipitates far earlier than CH3NH3Cl because of the better solubility of MeAm*HCl - and it does so when being concentrated and cooled as well as when acetone is added.
By doing several "partial extractions" like described, all ammonium chloride should theoretically have completely precipitated, as soon as methylamine hydrochloride crystals start crashing out.

And through diluting the mother liquor several times with a solvent forming an azeotrope with water/HCl, it should become almost water-free without having to heat it very much, a thing also called "azeotropical drying". IPA forms an azeotrope with water; and although having no proof for it, I'm quite sure that acetone carries lots of aequ. HCl with it when being distilled from aequous, acidic HCl salt solutions...
But after some conversation with other bees, I'm no longer sure about the azeotrope drying - as MeAm*HCl is pretty soluble in IPA, and I suspect that many HCl salts in fact hold back HCl while allowing water to evaporate, thus HCl concentration rises, and solubility of MeAm*HCl is increased...(contrary to what is desired!)

anyway: IPA carries at least something with it when being distilled, and it simply evaporates much quicker upon vac distillation than aequ. HCl for example...)

So far the theory on the workup.





Results and discussion...

Well - since I spilled the last washings (LOTS of IPA/acetone/MeAm*HCl on the lab floor - cough...), and since I freebased the product directly without proper isolation/weighing, the yields obtained are a bit vague... ::)

But as MeAm has a higher pKb than NH3, some residual NH4Cl shouldn't make any difference when the product is to be used in reductive aminations (regardless whether Al/Hg or othe reduction methods) - methylamine is a stronger base and displaces ammonium ions, so if the excess of amine is big enough, the only amine reacting should be methylamine - in theory. (you see abolt I AM capable of admitting if I was wrong - at least if I REALLY was..) So probably the legthy workup isn't required at all - but I just like having clean products, as I can be sure the reason for failures is not lack of purity but rather my skillz... ;)

{this post is still under construction  ;) }


armageddon

  • Guest
another variation - part III
« Reply #116 on: August 05, 2004, 09:56:00 PM »
I can tell you, never before have I spent that much time in my lab just to complete one synth...

Anyway: the resulting MeAm/MeOH solution (minus the small amount that was lost because of a minor suck-back while gassing) was thoroughly dried over 4A molecular sieves while keeping in the fridge, and 20ml of this dried solution (volume 423ml in total) were diluted to 60ml. This was divided into two portions and each was triturated with aequ. 2N HCl using phenolphtalein indicator, until color disappeared.



Results:

          first trituration: 8.7ml 2N HCl  -> 0.0174 mol CH3NH2(g)
         second    "      : 8.65ml 2N HCl -> 0.0173 mol CH3NH2(g)

    0.0173 mol  +  0.0174 mol  /  2  =  0.01735 mol => 0.5389g CH3NH2 per 10ml undiluted solution

(meaning a concentration of roughly 5.4% w/v of methylamine/methanol)

    423ml * 0.05389 = 22.79 grams methylamine(g) in total

For better comparison: this equals 49.55 grams MeAm*HCl or a molar 45 percent yield, calculated from NH4Cl (which is the limiting reactand I think). Not too bad, dare I say - taken into account my usual spillages and other losses during gassing... ::)  8)

Now you all are invited to happily tear to pieces what I described - I don't care anyway... :)

BTW does anybody know if it is possible to distinguish between primary and secondary (and maybe tertiary?) amines using Nesslers reagent? Or anything similar? Any input would be greatly appreciated...

Greetz, A


lugh

  • Guest
Hinsberg Test
« Reply #117 on: August 06, 2004, 03:21:00 AM »
The Hinsberg test is the recommended procedure, since the nitrous acid test can produce carcinogens of unknown potency   ;)

Procedure

To 0.3 mL or 300 mg of unknown in a test tube, add 5 mL of 10% NaOH solution and 0.4 mL of benzenesulfonyl chloride. Stopper the test tube, and shake the mixture vigorously. Test the solution to make sure that it is still alkaline. After all of the benzenesulfonyl chloride has reacted, cool the solution and separate the residue, if present, from the solution. Test the residue for solubility in 10% HCl solution. If no residue remains, then treat the solution with 10% HCl solution and observe whether a precipitate forms.
Positive Test

1° amines - dissolves in base and precipitates from acid is a positive test.

2° amines - precipitates from base and no change from acid is a positive test.

3° amines - precipitates from base and dissolves in acid is a positive test.

Complications

Amphoteric compounds give erroneous results.

Some sodium salts of benzenesulfonamides of primary amines are insoluble in the Hinsberg solution and may appear to be secondary amines.

Some tertiary amine hydrochloride salts are insoluble in dilute HCl and water and may also appear to be secondary amines.


http://www.chemistry.ccsu.edu/glagovich/teaching/472/qualanal/tests/hinsberg.html



8)


armageddon

  • Guest
hm...
« Reply #118 on: August 06, 2004, 04:25:00 AM »
Let's say one poor bee hadn't any benzenesulfonyl chloride lying around, but some HNO3 - and is hopelessly impatient but still very brave and doesn't fear carcinogens... :)

How would the nitrous acid test look like? (just out of pure interest of course!  ;) )

(thanks anyway for your "Hinsberg" response Lugh!  8)  Seems like another versatile reagent I'll have to buy someday...)

Greetz A


lugh

  • Guest
Qualitative Tests
« Reply #119 on: August 06, 2004, 04:35:00 AM »
Dr. Glagovich has entire page devoted to the various qualitative tests:

http://www.chemistry.ccsu.edu/glagovich/teaching/472/qualanal/tests/tests.html



Why don't you just bookmark it and start studying?

:P