Author Topic: methylamine synthesized ala Bright Star´s:it´s good enough? (Read 1849 times)

jon · « **Reply #40 on:** April 26, 2011, 04:14:59 AM »

you don't need a condensor just a line of tubing sealed with ductape to a beer bottle in a pot of boiling salt water (boiling at 106) connected to an aspirator running the *slightest* vacum does the best job of making methylamine hands down because it converts all the formalin to methylamine it does'nt come back as dirty yellow it comes back white you don't even have to recrystallize it it's less hygroscopic because it's pure easier to do things right in the first place.
than be lazy and work twice as hard in the end cleaning the shit up.

salat · « **Reply #41 on:** April 27, 2011, 04:00:21 PM »

why people don't do it this way

Too much vacuum you wind up pulling the product out, but without it more stuff (like formic acid, CO2) stays in the pot to interfere with the reaction.

Vacuum is done to increase yields. When you spend 2 days working a reaction it makes sense to get as much as you can out of it.

I haven't tried jon's reaction but it sounds like it's got all the right ingredients. Going to ask xBee to try increasing the temp a bit next reaction to see if that helps. Last batch he made he got 5 mol methylamine with a light yellowish tinge from 4 mol hex. jon's method sounds like a matter of having hit just the right conditions to get everything working right. One big pot probably does make it harder to get it done. All that fancy lab glass fucks us up!

We don't drink so I guess I could get root beer bottles....

Salat

Methyl Man · « **Reply #42 on:** April 27, 2011, 07:12:23 PM »

Couldn't one, if they chose to use lab glass, hook up a vacuum valve type thing inline within the tubing to the vac pump, and use it to dial in an amount of vac that is just right? What are those called again, pin-valves?

Seems like jon's way requires some way of dialing in a slight vac, so why not (if using a strong vac pump) do it with precision. Don't they make them with vacuum gauges as part of the thing too? I could swear I've seen those. With a gauge, one could reproduce the right vac on subsequent operations even more easily.

Oerlikon · « **Reply #43 on:** April 27, 2011, 07:34:49 PM »

Jon is never THAT specific,his methods work well even with totally amateur equpment.
I think that "just right" vaccum is when reaction mix bubbles like freshly opened soda drink.

jon · « **Reply #44 on:** April 27, 2011, 08:58:59 PM »

the just right vacum is done with an aspirator easy to dial that down just lessen the flow of water.
my favorate part of that reaction is cracking the 32 or 40 ounce what have you beer bottles open and guzzling the shit down.
you'll know when the vacum is spot on because all the co2 can be seen bubbling off the top not the bottom that was the idea to pull co2 out to drive the reaction forward and it works dandy just gauge it by eye.

salat · « **Reply #45 on:** April 27, 2011, 09:55:34 PM »

I have a setup on my vac as does xbee - a needle valve connected to a tube of drying agent and a manometer that allows us to control the vacuum pretty precisely. I'm just trying to figure out why jon's method works so well opposed to what xBee is doing which is pretty close.

xBee says the reaction mixture never got close to 106 so it may be that he should increase heat, but that doesn't sound right either. Heating in a 3 or 5 liter flask is more likely to have hot spots and be uneven, although xBee says he's got really strong stirring so that shouldn't be it.

Salat

jon · « **Reply #46 on:** April 27, 2011, 10:14:10 PM »

you should use a saturated salt water bath because the temperature goes between 104-106 106 being optimal you can always tell you have achieved the optimal temperature when co2 evolution becomes vigorous.

akcom · « **Reply #47 on:** May 12, 2011, 05:17:22 AM »

not to suck anyones dick here or anything, but jon is a god damn genius. this salt water bath is perfect, internal temp of the reaction is 106C on the spot.
jon suggested a 4:1 molar ratio, but I ended up using 110mL 31% HCl + 41g Hexamine based on RoundBottom's notes. Assume 7% of your hexamine is binder if you're using tablets.

I was not comfortable using a beer bottle for the first time. I couldn't find a clear one, and I wanted to be able to see the reaction. If you're like me just set your flask in a small pyrex bowl full of saturated salt solution, wrap the bowl in Al foil and tent it over the neck of the flask. This will reduce the amount of steam you lose, but you will have to add a little water every couple hours. Connect your aspirator and turn it on once CO2 starts to evolve (when the bath temp hits 85-90C).

My aspirator on an aquarium pump was not strong enough to pull a good vacuum for this reaction. The CO2 was bubbling from the bottom instead of the top. Next time I'll try doing it straight from a faucet.

Hexamine & HCl were added to a flask. The flask is swirled occasionally by hand to help dissolve the hexamine. The temperature was brought to 106 over a period of 1 hour. I fiddled with having my aspirator running during this period, but it didn't really seem to be making a difference so I finally just left it off and set up for distillation. After about 4-5 hours of reacting CO2 stopped evolving. Some distillate had obviously been sucked down the aspirator because only a very small amount of liquid came over once the solution was at 106C. As a note the solution is almost colorless, none of the yellow people talk about. Its much closer to the color of dilute muriatic acid.

I will finish this once I separate off the AmCl

jon · « **Reply #48 on:** May 12, 2011, 06:42:49 AM »

you need to dilute that acid you can't just use it straight you can but it's not advisable.
use elusis's dilution in the methylamine from hexamine faq
i'm not a genius i just spent a long time doing the same thing over and over again.
let that cool all the way to room temp or you'll be filtering endlessly.
use a fan to cool it quickly.
also use your nose it should smell of rotten pussy with no detectable hints of formalin (sorry ladies)

Shake · « **Reply #49 on:** May 12, 2011, 07:59:57 AM »

Quote

not to suck anyones dick here or anything, but jon is a god damn genius

It is like the movie twins, only im danny devito

Hey ackom, nice post bro. people seem to take results posting for granted, but for non chemists or people who havnt walked the path before, these write ups are everything.

Cheers

Shhhake

shroomedalice · « **Reply #50 on:** May 12, 2011, 10:16:47 AM »

another reason to use a slight vacuum when making this amine from hexamine is that it
slows down the dimethylamine being made there for creating more mono methylamine.

this will make it so you dont loose as much weight when washing with dry DCM
to remove the dimethyl amine impurity that arises from making this amine through formaldehyde
and ammonia.

sassa · « **Reply #51 on:** May 12, 2011, 03:39:37 PM »

NO SOURCES

READ THE RULES :

http://127.0.0.1/talk/index.php/topic,369.msg3325.html#msg3325

SORRY MODERATORS!....My most sincere excuses... I was doubting if i can post it or not....

jon · « **Reply #52 on:** May 12, 2011, 09:08:59 PM »

actually at 106 no dimethylamine is made

no one in thier right mind would buy that.
some people are sting op's others are genuine outfits that sell hot chemicals for a profit.
the best way to find out is to order a non-suspicious item from them and see how they declare it to customs and where the package came from.

RoidRage · « **Reply #53 on:** May 12, 2011, 09:09:18 PM »

Quote from: sassa on May 12, 2011, 03:39:37 PM

hXXp://cgi.ebay.com/Methylamine-hydrochloride-95-500g-Lab-Reagent-/330553241486?pt=LH_DefaultDomain_0&hash=item4cf6822f8e

***ADD TO WATCH LIST***

Wonders if it will last long ? Technically, it's perfectly legal

Wonders if they're willing to mislabel too

jon · « **Reply #54 on:** May 12, 2011, 09:24:03 PM »

only one way to find out, they are purportedly from overseas but that could be a ruse too.
so order something benign say you don't want to pay hazardous material duties and see what they say.
i've seen digs like this before.
just see where they do business off ebay so the pigs aren't privvy to your business.

sassa · « **Reply #55 on:** May 12, 2011, 09:29:28 PM »

haha...only posted for fun...
..I discovered that days ago looking for calcium sulfate,and i´m sure he doesn´t carry it days ago,because i was revising all items for sale,......but seems seller it´s a reputable e-seller from China,with lot of happy customers,and auctions are private,..have and advice on the bottom of the auction to ebay´s advertising to not delete items because there are not listed as scheudeled on lot of countries...It´s usual for people from usa,think on that as a crazy thing,but on other sites of the world,buy this can be not too much safe, but perfectly legal.
And carries too diethylamine,ethylamine,.....

.
  Something says to me this seller knows what he sells,and it´s very posible he acced to mislabel the packages if customs on the destin country are too much hard....
   Posibly too,ebay make the posibility of order to a different adress,include far a lot from original adress,pay with another ebay acount,another paypal acount,so....
   I will not recomend anybody buy it of course!,but i believe can be easy to get to people from some countries talking a little to the seller,.....
i posibly will buy him some Calcium sulfate,and will ask for some "adjusting" on packages information because customs,...so i will see how it works.Information coming soon....

jon · « **Reply #56 on:** May 12, 2011, 09:41:49 PM »

yeah like i said there are a lot of foreign outfits that advertise there the trick is to find out where they do business off ebay because private does'nt really mean private.

salat · « **Reply #57 on:** May 13, 2011, 01:22:14 AM »

A company with that name was operating out of North Carolina a while ago - they seemed suspicious to me based on what they were selling. Reagent something - makes me think some agents think they are being clever.

Salat

jon · « **Reply #58 on:** May 13, 2011, 02:44:13 AM »

that's what they do they pose as an overseas outfit to make people comfortable.
what did you do look them up in whois?
they say are in henderson, nevada
you know you can look at those websites that the dea run like that one for example and learn a lot about what they are looking at.
suprize! suprize! SOCKS error trying to get to them behind tor, these guys really are fishy.

akcom · « **Reply #59 on:** May 13, 2011, 03:47:51 AM »

The solution was left to cool and the ammonium chloride was filtered out. The solution then reduced to dryness under vacuum. Vacuum was removed, MeOH added, and reflux attained. The MeOH was decanted, let slowly cool to RT, then put in the freezer.

I made the mistake of only cropping out the AmCl once, not twice. After recrystallization from MeOH I got a lot of translucent plate-like crystals, but also a lot of white powder as well. Added it to some NaOH solution and all I smelled was ammonia :\ Seems like I should have either reduced the solution w/o cooling until AmCl precip out THEN filtered, or just reduced the solution half way and filtered a second time. Just posting this here so no one else makes the same mistake I did.

Author Topic: methylamine synthesized ala Bright Star´s:it´s good enough? (Read 1849 times)

jon

Re: methylamine synthesized ala Bright Star´s:it´s good enough?

salat

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Methyl Man

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Oerlikon

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jon

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salat

Re: methylamine synthesized ala Bright Star´s:it´s good enough?

jon

Re: methylamine synthesized ala Bright Star´s:it´s good enough?

akcom

Re: methylamine synthesized ala Bright Star´s:it´s good enough?

jon

Re: methylamine synthesized ala Bright Star´s:it´s good enough?

Shake

Re: methylamine synthesized ala Bright Star´s:it´s good enough?

shroomedalice

Re: methylamine synthesized ala Bright Star´s:it´s good enough?

sassa

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jon

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RoidRage

Re: methylamine synthesized ala Bright Star´s:it´s good enough?

jon

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sassa

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jon

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salat

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jon

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akcom

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