AllChemystery - 2016-08-29
in this video i prepared some 5_aminotetrazole via the method outlined in U.S Patent 5,541,682 . this method has its advantages over the similar schtolle method in the way that little deadly HN3 is produced making this method much safer. you also do not need aminoguanidine bicarbonate which is hard to buy and a difficult and drawn out process to make yourself. we use Dicyandiamide {2-Cyanoguanidine) instead and this was easier to find from a chemical supplier and reasonably cheap in high purity.
Firstly though i needed more NaN3 and show making this also, but from the beginning: Hydrazine sulfate and isopropyl nitrite.
So the Sodium Azide was made and the synthesis can go ahead as planned. The reagents needed were:
1. 55g Boric Acid
2. 50g Dicyandiamide (2-Cyanoguanidine)
3. 38.71g Sodium Azide
4. 500ml distilled or deionised water
These reagents were:
1. 55g Boric Acid
2. 50g Dicyandiamide (2-Cyanoguanidine)
3. 38.71g Sodium Azide
4. 500ml Distilled or deionised water
These reagents were placed into a single necked 1000ml flat bottom flask and fitted with a reflux condenser which had circulated iced water to cool it. Stirring was started and the flask heated to reflux.
once the solution was boiling the water pump was turned on the condenser and the refluxing was done for 24 hours.
At the end of this time 75mls of HCl was added while the flask was still hot and then allowed to cool before being placed in the refrigerator for 2 days to fully precipitate the desired product.
This was filtered and recrystallized from hot water yielding a nice crop of snow white plate like crystals of 5-Aminotetrazole.
I Decided to further purify about half of the yield to get extremely pure crystals to again make Copper Nitrotetrazolate, which i did yesterday with brilliant results in very high yield.
More to follow...
possibly the most dangerous video on youtube. Thanks to democracy
Great video. Thanks for putting this together. I don't have an interest in tetrazoles but always good to see a nice preparation of such basics as hydrazine and isopropyl nitrite.
j_sum1 thanks! It was a memorable synthesis. Getting those nice pure crisp white crystals in decent yields is always rewarding. Especially after doing the other slightly more involved synthesis for lower yield of lower quality product.
The forming of crystals and recrystallising for high purity is probably my favourite thing about most synthesis I attempt.
What is your main interest in chemistry?
Nice work!
Great job!
Great video!
No demos of you uaing it?
Will you make a movie on processing 5-Aminotetrazole into Tetrazole?
It could be done as is described in this paper: R.A. Henry, W.G. Finnegan: An Improved Procedure for the Deamination of 5-Aminotetrazole in J. Am. Chem. Soc. 76 (1954) 290–291, DOI:10.1021/ja01630a086
WOW!!!!! I just checked the refrigerator, my solution has only been in there for 30 min since finishing reflux and it is one solid mass of pure white crystals. I mean the entire liquid has been replaced with crystal, is that normal?
So I just broke them up and there is still water in there but a ton of crystals so far. They look great.
wesson smith you’ll need to recrystallise it for the nice plate crystals. Is so satisfying after so many steps
Where did you get the dicyanamide from? I've been looking for a source, but haven't been able to find anything at a reasonable price.
Bill Smathers
Thermal decomposition of calcium cyanate, hydrolyze, then alkalize.
i m waiting for the reply
chemistry what did you need to know?
@AllChemystery ,Thank for your response. I used 1-cyanoguanidine as dicyandiamide, I used values as same as patent without scale up. Reflux condition: oil bath, Temp.:95 C. so I did as you.that means I added warm dist. water to solids, but I turned on the condenser first not like you(you first heated to boil and then turned on it). I observed the solids dissolved in the water and colorless solution obtained. I know as you mentioned and also patent structure, it should have turned orange. So I ask you to,1- more describe your reflux condition, 2-and tell me that 1-cyanoguanidine and 2-cyanoguanidine have same performance or not? and why turn to orange?(NaN3?)...Thanks again.
@AllChemystery, Hello there!!!!!!!!!!! I am waiting....
@AllChemystery, are you there?why didn't you answer?it was not POLITE.
chemistry sorry. Life is busy right now. As far as I can see you are starting with 1- Cyanoguanidine. You need 2- cyanoguanidine. Your other conditions seem correct.
What sensitivity difference did you notice between Sodium Nitrotetrazole and Silver Nitrotetrazole?
wesson smith silver has greater overall sensitivity but I think there’s more power in the sodium
Did you make 2-Cyanoguanidine or buy it? made from calcium cyanamide , water and dry ice (CO2) first to make cyanamide and after 2-Cyanoguanidine . I believe that cyanamide with ammonium nitrate if when intermolecular mixture may be a powerful explosive mixture, although cyanamide is unstable due to its standard enthalpy of endortermic formation such as Hydrazine , i need try it !!!
Energetics Tests I bought it. Easy that way.
Very nice video.
What liquid did you use to further purify the 5-ATZ, H2O or Acetone? If H2O was it warm? Thanks. FYI I am currently refluxing my first batch of 5-ATZ using your modified Thiele method.
Water. You would need to work out solubility of ATZ in cold water to not loose too much. It’s fairly soluble in hot water though. Not too muofch or crystallisation will be slow. Toy may need to seed it with a glass rod. It’s very pretty once it begins if you have the right level of ATZ saturation
@AllChemystery Great, thanks. My current reflux at 1hr looks perfect. 1 more hr to go:) FYI I am using the Aminoguanidine Bicarbonate I purchased on eBay. So far so good:)
What chemistry is this compound used for?
generally it is a precursor some interesting nitrogen packed compounds with bad tempers.
AllChemystery amen to that lol
things go boom
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So here is my current mix. As you can see it's quite impressive. My goal is to use Sodium Nitrotetrazole dissolved in acetone and add it to the already pressed carrier powder, this way I am not messing with the Sodium Nitrotetrazole once it's dry. I want to use Sodium Nitrotetrazole instead of the other special ingredient, the one that melts at 61° C. because the Sodium Nitrotetrazole has a much better thermal stability and will be considerably more powerful. If it works then we have a "green" detonator with a +200°C operating temperature, which is fuse sensitive and doesn't require a secondary. Very Safe and easy to load.
https://youtu.be/ufdyrfMo_nM
ecstasy.apostasy - 2019-04-16
OI YOU MADE CuNTZ TOO?
J H - 2020-01-08
He can make CuNTZ any damn time he pleases!