I have always had trouble preparing this. As we know its a protic base, which can indeed promote alkene formation rather than an alcohol iin various condensation type reactions. I have heard of using stiochemetric amounts of GAA or conc acetic acid with ammonium hydroxide, or just get to a neutral point, and as one is evaporating slowly allowing Nh3 to be channeled across the surface of the mix; (This is hearsay, so I may indeed have this wrong)This seems an annoyance, so rather than trying that method, I thought I would ask the many schooled members of the Vesp, for any tricks of the trade, with respect to what surely is an acid/base reaction- albeit between 2 species with different vapor pressures/qualities etc, I an wanting this as a solid, that i can put in a vac desiccator, BTW, if any Aus member has surplus (INFORMATION THAT IS) perhaps you could pm me, rather than clutter up this simple question of a thread.

2bF

Do you think directing NH3 as your evaporating, say on a water bath, has merit. or just monitor pH, and if it gets a little lower due to the release of NH3, add a liilte to compensate. Perhaps a water bath is problematic, and best just left to evaporate naturally, and then put in VAC des./// thanks for your reply btw

If you can produce NH3 like by way of decomposition of urea (best, no H2O)  or base + ammonium salt.. you could just direct that gas into some pure GAA - keeping it a bit warm and adding a strong excess of NH3 should yield the ammonium acetate with much problem, right?

NH3  + CH3COOH => CH3COONH4

It doesn't even produce water as a by product or anything. You'd have problems with it at the end though - perhaps some of the acetic acid would be trapped with the ammonium acetate crystals. This could be remedied by chopping/spreading about the bulk powder and allowing it to evaporate.

Note: Unless you want suck back, don't dip the NH3 tube into the GAA - perhaps have the GAA on a magnetic stirrer, and the NH3 tube above it, sealed off. This will create a lower pressure in the urea decomposition flask, and probably help things along?

Awesome, report how it goes
Seems like suck back is something to fear.. so just a reminder to avoid that. I can't imagine how fast NH3 would dissolve in GAA.

acetamide can be turned into ammonium acetate cant it? I guess maybe not.

Urea + GAA, heating and refluxed can yield acetamide crystals in the reflux condenser so I have heard. Someone over at SM claimed to have great success with producing acetamide this way.

You can add ammonium carbonate to glacial acetic acid to obtain ammmonium acetate    You need to dry it under a vacuum, keeping the temperature low enough to avoid decomposition:

The route to CH3CONH2 does proceed thru CH3COONH4 on at least one occasion.  Various literature states that one method used in preparing acid amides or in this instance more specifically CH3CONH2 is by the dehydration of its corresponding ammonium salt.  So imo it would be possible to utilize 1 of the 2 more well-known routes used when discussing routes to  CH3CONH2.  One thinks this is somewhat similar to Lugh's suggestion however in this process dehydration is accomplished within the synth itself (unless I am missing something???) either way you would need: 15g of Ammonium carbonate, 15 g.; acetic acid,  and a 50 ml.of GAA.

Add 15 g. of finely powdered ammonium carbonate gradually to 50 ml. of glacial acetic acid contained in a 150 ml. rb flask, shaking the mixture during the addition to ensure a steady evolution of carbon dioxide. When all the carbonate has dissolved and the evolution of carbon dioxide has ceased, proceed to setup your flask for reflux by utilizing an appropriate open-air condenser, boil the solution gently for 3o minutes, when the dehydration of the ammonium acetate will be complete. Now remove the condenser and fit a fractionating column to the flask (at this point the literature which is a bit dated does make strong mention of the need for an efficient fractionating column. They proceed with providing dimensions for fabricating such devices, which imho probably dates this synth well before many of our equally effective modern day devices not only became more easily accessible but also helped establish standards, therefore an abbreviated version of this dialogue equates to an efficient column with the "height of about 12 cm. is used". Now distill the liquid through the column very slowly (to give about 1 drop of distillate every 3 seconds) until the temperature reaches 17o°: it is very important that this operation should be carried out slowly in order to distil over as much water and excess of acetic acid as possible, and so to leave almost pure acetamide in the flask. Without delay, pour the hot molten acetamide into a small (5o ml.) distilling-flask, and attach the sidearm of the flask to a short glass tube (about 3o cms. long and t2 mm. internal diameter) to act as an condenser. Distill the acetamide carefully at such a rate that none escapes condensation, and that none crystallises while still in the condenser. Collect the fraction boiling between 215° and 225°  Yield, 15 g.

The later part of this synth. would obviously be omitted for your needs however should one not have a problem with either the availability of reagents or the requirement of a little manual dexterity by shaking a container followed by the ability to set-up a simple reflux apparatus, then hopefully this is what you are looking for. Hey I am still looking for one on ph strips so dont feel bad.

Not sure if the Urea route mentioned would be viable in acquiring  CH3COONH4 however another type of ammonium does turn up in the Urea method and that is NH4NH2CO2 however since one has recently become a die-hard hofmann fan and loves the idea of synths starting from the floor up, then you could safely assume he would jump at the chance and say something like;

In regards to acetamide via urea, one could try placing 25 g. of glacial acetic acid and 25 g. of urea in a 100 ml. triple neck rb flask. Fit the center neck with an appropriate air-cooled condenser set for reflux. In either side-arms insert your thermometer so that the bulb in the mixture and 1 cm. from the bottom of the flask, close off the remaining neck with appropriate device such as a rubber septum. Heat the mixture gently either on a wire gauze or in an air bath. When the urea melts, shake the flask gently in order to mix the acid and urea layers. Gradually raise the temperature so that the liquid just refluxes in the condenser. The temperature is about 150° after 30 minutes and a whitesolid (probably ammonium carbamate) commences to form in the condenser : push the solid back into the flask by means of a stout glass rod when complete blocking of the condenser appears likely. Continue the heating until the temperature of the liquid is 195-200° ; this temperature is attained after a heating period of 3-3.5 hours. Both carbon dioxide and ammonia are evolved. Allow the apparatus to cool and rearrange it for distillation. Heat the flask slowly at first ; some ammonium carbamate first sublimes into the air condenser. When the acetamide begins to just reach the condenser, stop the distillation momentarily, replace the condenser by another of similar size and continue the distillation. Collect the acetamide at 200-216° (most of it passes over at 214-216°) ; if it crystallizes in the condenser, it may be melted by the cautious application of a flame. The yield of almost pure, colourless acetamide, m.p. 80.5°, is 22 g.


much love
mez

You can add ammonium carbonate to glacial acetic acid to obtain ammmonium acetate    You need to dry it under a vacuum, keeping the temperature low enough to avoid decomposition:

I only got ammonium bicarbonate, would that suffice or should I put that in H2O solution the Hydrogen may bubble of leaving NH4+ and CO3-2 and if I evaporated this slowly - with little heat then ammonium carnonate would come out of solution. I am saying this with respect to VESP'S idea of doing this with NaHCO3  

i am also stating this re ammonium acetate by using ammonium carbonate and GAA, as whats been stated

yep correct, and yep Ill stop- another spoonful pls- and use whats been given to me,

I just wrote it out in front of me, which simplifies it to the acetic acid protonating the HCO3 thus forming carbonic acid,
that will dissociate to CO2 and H2O, and if this is done in a vacuum these two will be driven of. So sorry, its me being lazy I
suppose, I find such resistance to think at times, It could be the water, they putting something in it, so we become dumb.
Im fucking serous. It wouldn't surprise me in the least. JUst pacify the fucks, with DUMB FLUID. What I questioned was basic acid base
chem, and I didn't see it.  

and even now I better double check it, SEE dumbness kickin in,

YOur probably right the b.p. of water and acetic acid is problematic, I think ill go with dry NH3 into dry GAA and take it from their. Ill look at all this later, Ive got bussiness that I initially thought was at 9, and its now at 1.30pm, so got to go, Thanks lugh. btw.