Can I use this for acetylations?

[Dr.Mirakulix]

Hello folks,

I'm in need for an acetylation agent, acetic anhydride to be precise (I don't want to mess atound with unnecessarily toxic stuff like acetyl chloride).
Anyways, while looking around I found this product (and only this product):

(The title says 'Acetic acid 100%' in German)

Is this the same as AA? It's a regulated substance in my country, but only in the generous amount of 100 l and upwards. Nevertheless it seems quite difficult to source some here. Even glacial acetic acid is kinda rare to legally obtain.

Long story short: Is this product acetic anhydride and usable for acetylations?

Also: Is it safe to order this or will this instantly put any buyer on some kind of most-wanted-by-goverment list, like a honey pot ? Should I take any elaborate and special precautions before buying this product?

Thank you in advance!

 

[archae]

This isn't acetic anhydride. It's acetic acide. Different chemicals. If you are in doubt, you can check the CAS number of the compounds, as this completely disambiguate the names. If they have the same CAS number, they are the same compound.

What is it you want to acetylate? Sometimes GAA can be used. If it's morphine, it might be possible to use this when adding sulfuric acid as a catalyst, but this route isn't very well described in the litterature

 

[Dr.Mirakulix]

This isn't acetic anhydride. It's acetic acide. Different chemicals. If you are in doubt, you can check the CAS number of the compounds, as this completely disambiguate the names. If they have the same CAS number, they are the same compound.

What is it you want to acetylate? Sometimes GAA can be used. If it's morphine, it might be possible to use this when adding sulfuric acid as a catalyst, but this route isn't very well described in the litterature

archaeHello and thanks for your reply! Oh that's sad. I guessed it had to be anhydride because it's 100% pure but that seems to be an error in my thinking. I thought 99% = GAA, 100% = AA?

Yes I wanted to acetylate morphine (morphine base extract to be completely precise). Thank you for the Tipp! I can get my hands on some GAA, only don't have an idea about the sulfuric acid? It seems it needs someone to experiment if this isn't documented well. ;-)

Edit: My research seemed to show that this acetic acid 100 % is in fact GAA. So I'm going to buy it either way and look out for a usable catalyst for the reaction.

 

[G.Patton]

Hello and thanks for your reply! Oh that's sad. I guessed it had to be anhydride because it's 100% pure but that seems to be an error in my thinking. I thought 99% = GAA, 100% = AA?

Yes I wanted to acetylate morphine (morphine base extract to be completely precise). Thank you for the Tipp! I can get my hands on some GAA, only don't have an idea about the sulfuric acid? It seems it needs someone to experiment if this isn't documented well. ;-)

Edit: My research seemed to show that this acetic acid 100 % is in fact GAA. So I'm going to buy it either way and look out for a usable catalyst for the reaction.

Dr.MirakulixHello. As @archae saide they are different substances. AA is abbreviation for Acetic Anhydride. GAA is glacial acetic acid (99% acetic acid).

 

[Dr.Mirakulix]

Hello. As @archae saide they are different substances. AA is abbreviation for Acetic Anhydride. GAA is glacial acetic acid (99% acetic acid).

G.PattonHello and thank you for the clarification! So basically that means I have to use what I can get here and (this was my original plan) go for synthesizing 6-MAM with Glacial acetic acid.

About the catalyst: Do you know if one could use any alternative catalyst instead of sulfuric acid (maybe HCl 37%?) The only way I know to source it OTC would be battery acid and I would not feel well about using that on smth that's meant for human consumption. And buying it in bulk from China seems no good solution, too, as I would need only a few mL. :-/

 

[G.Patton]

Hello and thank you for the clarification! So basically that means I have to use what I can get here and (this was my original plan) go for synthesizing 6-MAM with Glacial acetic acid.

About the catalyst: Do you know if one could use any alternative catalyst instead of sulfuric acid (maybe HCl 37%?) The only way I know to source it OTC would be battery acid and I would not feel well about using that on smth that's meant for human consumption. And buying it in bulk from China seems no good solution, too, as I would need only a few mL. :-/

Dr.MirakulixAs far as I know, you can get 3-MAM from morphine. 6-MAM can be obtained from heroin. I haven't found any information about alternative ways. I think it is impossible to use HCl in this synthesis as catalyst.

 

[OrgUnikum]

Acetylation with acetic acid produces the so called "tar heroin". Acetic Anhydride is easily made from Acetylchloride, It is just adding the chloride to GAA and distilling IIRC, you find more detailed information in the sciencemadness.org chemistry wiki, with links to related threads.
Acetylchloride from Poland, I guess you know the places. Might work with Benzoylchloride too, thats available in the Netherlands. Shop should be known.

H2SO4 can be replaced in this kind of reactions by metaphospohoric acid, which can be bought or is made by heating H3PO4 to about 150 °C for a prolonged time until only a crystalline mass is left which consists if one waited long enough predominantly of metaphosphoric acid. It works very well and clean as catalyst but it takes time to do its job, days.
Other catalysts might be tosic acid (anhydrous) or triflic acid.

 

[Dr.Mirakulix]

Acetylation with acetic acid produces the so called "tar heroin". Acetic Anhydride is easily made from Acetylchloride, It is just adding the chloride to GAA and distilling IIRC, you find more detailed information in the sciencemadness.org chemistry wiki, with links to related threads.
Acetylchloride from Poland, I guess you know the places. Might work with Benzoylchloride too, thats available in the Netherlands. Shop should be known.

H2SO4 can be replaced in this kind of reactions by metaphospohoric acid, which can be bought or is made by heating H3PO4 to about 150 °C for a prolonged time until only a crystalline mass is left which consists if one waited long enough predominantly of metaphosphoric acid. It works very well and clean as catalyst but it takes time to do its job, days.
Other catalysts might be tosic acid (anhydrous) or triflic acid.

OrgUnikumThank you for your reply!

In search for more information about this reaction, I found some reports of people sucsessfully using Glacial acetic acid with Natrium acetate as catalyst to form 6-MAM from morphine in another forum. I want to experimentally try out this Route, but I was wondering and trying to figure out how much of the Natrium acetate would be needed and how one should go about removing the catalyst from the final product. The people over there told that you can stochiometrically calculate how much Natrium Acetate is needed, but I've got to admit, I don't know where to start about this.
Sorry for so many newbie questions, I hope I'm not going on your nerven already and that someone can help me out.

 

[OrgUnikum]

You would save yourself a lot (really a lot) trouble and pains if you would concentrate on sourcing acetic anhydride or the chemicals needed to make it. This is caused by the simple fact that acetic anhydride is the reactand which allows you without serious experience with chemistry to make Heroin from Morphine.

In 20+ years of on and off dabbling in drug-chemistry I changed from somebody who suffered the delusions everything should be OTC to somebody who rather spends more time sourcing high quality precursors and chems as even with those at hand and a decent understanding of the chemistry and good lab-practice its more often then not still not nearly as easy as it looks.