Sciencemadness Discussion Board - MeAm from HMTA (hexamine)

MeAm from HMTA (hexamine)

Clandestiny - 6-11-2018 at 10:12

Good day all,

Clandestiny would like to report what he has so far for his first attempted synthesis at MeAm*HCl. The goal here was to decompose the HMTA (hexamine) to formaldehyde and ammonium chloride through hydrolysis and subsequent reflux. Any criticism and advice is GREATLY encouraged/appreciated. Here is the rough lab write up and notes he took during the procedure:

@ 0900 - 179 grams of hexamine (camping fuel tablets) were pulverized with a mortar and pestle and added to a 1 L RBF.

@ 1015 - 88 mL of 18 megaohm water was stirred into the hexamine. About half of the hexamine had dissolved when 400 mL of concentrated (38%) HCl was added quickly to the RBF. Upon further reading, it seems that quick introduction of HCl is not recommended as it can lower yeild. Anyways, the mixture was stirred until 1050.

@ 1050 - All of the hexamine solid was successfully dissolved in the RBF. The reaction was noticeably exothermic, but nothing too warm. A few minutes after this, there was a rapid formation of white fluffy crystals forming in the flask, Clandestiny thinks this is NH4Cl.

@ 1100 - Reflux was set up in a peanut oil bath and run for 4 hours at 80-90 degrees celcius. An interesting note here is at 1152, the fluffy white solids went back into solution at 46 degrees C. Throughout the entire reflux, there was a substantial evolution of gas, which seems like H2 forming from the heated HCl. The amount of bubbles evolving never seemed to slow down during the entire process from here on.

@ 1600 - Standard distillation was setup with a liebig condenser. A submergeable pump was placed in a bucket full of ice water as a source of water flow as this reaction was taking place away from any sinks.

@ 1730 - Fluid started coming over at 103-106 degrees. What was strange about this distillation is that the speed at which condensation occurred was very, very slowly. It took about 20 seconds on average for each drop of distillate to enter the receiving flask.

@ 1930 - Distillation was still very slow, and it looked like there was only a measly 15 mL of distillate total after 2 hours. It was decided to end the distillation for the night as something seemed awry. Ideally, NH4Cl crystals should have formed as the distillation was coming to and end. The goal was to filter off the NH4Cl crystals after the distillation was complete, and then distill the filtrate to dryness (sublimation of MeAm). This, of course, did not happen.

@ the next morning - The reaction vessel was kept at slightly below room temp overnight, and the next morning half of the flask was filled with solid white crystals in a in a clear solution. This was akin to a super thick slush. Any thoughts or criticisms?

Texium - 6-11-2018 at 10:20

Criticism:

1. Drop the 3rd person. It's extremely tacky.
2. MeAm is not a valid abbreviation for methylamine. Say MeNH₂ if you must abbreviate.
3. You don't appear to reach any real conclusion.
4. The time intervals you break it up into are not relevant for the most part. Mention how long something was stirred/refluxed etc for instead, otherwise it isn't necessary.

Clandestiny - 6-11-2018 at 10:44

Texium,

Thanks for the information pertaining to post format and norms. And I did not reach a conclusion or ask specific questions. What I am more so curious about is the identity of the white solid that dissolved back into the solution as the temp was raised for reflux. Many of the posts I've lurked through do not seem to note this occurence.

fusso - 6-11-2018 at 11:19

Just judging from your username and wrong use of abbreviations/symbols, you look like wanting to become a drug cook. Don't make us feel like you're a drug cook if you don't have intention to become one.

morganbw - 6-11-2018 at 12:27

Quote: Originally posted by fusso

Just judging from your username and wrong use of abbreviations/symbols, you look like wanting to become a drug cook. Don't make us feel like you're a drug cook if you don't have intention to become one.

Just from my view, when you scold someone please, use the term (me or I), do not use the term "us".

I am one of us's and I will post my opinion when I get the urge. Please do not attempt to speak for more than yourself unless you provide some credentials that you may.

To the OP, search and study this forum a little more, there are given a few good methods from hexamine to methylamine.hcl, spread throughout this forum, as well as some other forums.

Methylamine.hcl actually does have uses beyond wanting to become a drug cook.

The white solid which dissolved back into the solution was probably Nh3Cl.

If by chance, you are, as insinuated by, (@fusso), attempting to be a drug cook, please be a good one with some ethics to as what you produce and purity.

[Edited on 11/7/2018 by morganbw]

Clandestiny - 6-11-2018 at 12:58

Quote: Originally posted by fusso

You do realize that methylamine can be used for a very wide range of organic applications, right? It seems to me you have reached a very narrow-minded conclusion as you ASSumed what my intentions where.

fusso - 6-11-2018 at 13:28

Quote: Originally posted by Clandestiny

Quote: Originally posted by fusso

Oops, not meant to accuse you, my bad

Assured Fish - 6-11-2018 at 13:33

Quote: Originally posted by Clandestiny

Quote: Originally posted by fusso

Twas an educated assumption he made, your user name is evident of it and you havent shown much of an understanding about what you are raeding, implying either its very early in your research stages or you care little for the details and just want to get to the end result.
This combined with the even more obvious, being that methylamine is a known scheduled drug precurser and probably the most imfamous drug precursor to boot.

Im not going to assume what your intentions are but this forum does not allign itself with doing chemistry purely for the sake of making money or getting high. You have walked in here with a name that screams drugs (this by itself is not a big deal) you have then made a first post that is telling of a typical drug cookery post.
You did all this and you not understand why you think it odd that people here are going to jump to these kind of conclusions.

Clandestiny - 6-11-2018 at 15:54

Ladies and Gentleman,

If this clears anything up, the username was inspired by an old computer game published in 1996 by Virgin Games....I was definitely expecting people to understand that reference. It's also funny as well because the program that was used to animate the characters was called "Amino"

As for end product, I am more so concerned with getting quality methylamine for photography development purposes. It is damn expensive to purchase Metol (4-(methylamino)phenol sulfate). This can be synthesized through hydroquinone and methylamine.

Is it too late to change my username?

j_sum1 - 6-11-2018 at 15:58

You can U2U woelen or Bert for a name change if you wish.

I have some metol if that helps. How much were you thinking of and where are you located?
Sorry -- I did not get the gaming reference either.

J.

fusso - 6-11-2018 at 16:17

Quote: Originally posted by j_sum1

Sorry -- I did not get the gaming reference either.

Me too, in 1996 I wasn't even born yet!

(In addition, if I were you, I would've corrected the wrong abbreviation in the post after someone pointed it out.)

[Edited on 181107 by fusso]

Clandestiny - 6-11-2018 at 18:39

J,

Thanks for the offer, it is greatly appreciated. For me, it's also not just about the end goal, but attaining the knowledge and competency to physically manipulate the world around me. I'm sure all of you can relate (otherwise you wouldn't be here). I will be giving it another shot after reading some more material.

As for being hostile to Fusso, I apologize.