12-10-02 12:05
No 388168
Jaws is planning to make some MDA with his pipe bombs, but has a couple concerns he wants to run by the HIVE first.
Jaws is going to still make his bromo with tech. Hbr in Gaa.
He then plans on putting about 300-400g of ammonium chloride into a gas generator bottle and adding aqueous lye to it to bubble ammonia gas through a tube fitted with an inline drying filter (filled with, dried in oven, epsom salt)and into some ice cold methanol or IPA(300ml) in a salt-ice bath. He is then going to mix this with 50ml of bromosafrole in a pipe bomb and heat for 3 hours at 130 degrees.
His questions are:
1)Is the ice-salt bath wich cools the methanol(or IPA) to about -5, suficient enough to catch all or most of the ammonia gas(wich jaws believes has a boiling point of -35)??
2) Is adding lye a suficient way of bubbling ammonia gas into methanol or IPA?
Jaws noticed that Agent Smith didn't use ice-salt bath. He just put 140g of ammonium sulphate fertilizer in a bottle and added lye to bubble it into COLD methanol. He claims this to have worked fine but jaws is curious.
3) Jaws also wonders why when you need 10 times as much ammonia gas in solvent as the amount of bromo compond being used, Agent Smith only used 140g of ammonium sulphate for 30g of bromosafrole?
Agian jaws is going to use ammonium chloride wich he is sure will work just as well if not better, but someone correct him if he's wrong.
THE BEST WAY TO AVOID BEEING STUNG IS TO BEE A BEE YOURSELF
(Hive Addict)
12-10-02 13:37
No 388182
Well, ammonium sulfate and ammonium chloride will work equally well in the gassing, but ammonium sulfate is much more otc than ammonium chloride, as it can be bought by the pound at your local plant nursery as a fertilizer.
It is seductive, way too seductive. -Eleusis
(Chief Bee)
12-10-02 22:51
No 388327
1) Yes, an ice-salt bath is enough, as long as you bubble the ammonia gas slowly through the solution. Heat is evolved as the ammonia dissolves, so without the cooling bath the solution would heat up, lowering the solubility of ammonia and you would lose (some of) it to the atmosphere.
2) Yes, certainly. You should fill the inline drying filter with NaOH or KOH though, as MgSO4 is not a very strong/fast dryiung agent.
3) The reason to use a large excess of ammonia to bromosafrole is to prevent two bromosafroles adding to one ammonia molecule (forming an inactive dimer). The larger excess of ammonia used, the less of your bromosafrole will be lost through this side-reaction. Without doing any experiments, its hard to say exactly how much excess is needed, but 10x excess is a good rule of thumb.
(Hive Bee)
12-11-02 14:50
No 388558
Thanks BIG GUY for the info.
Hey BIG GUY jaws was wondering, is he misunderstanding (10x MOLAR EXCESS).
Jaws always assumed that this meant 10x the amount in grams, but now he thinks maybe not.
He is kinda confused on this because all of the posts he's read on this reaction when the posting bee says 10x molar excess he will then turn right around and say (Agent Smith) that he uses 140g of ammonium sulphate fertilizer for 30g bromosafrole, (or Dr. Strangegloves)that he used 25g of methylamine with 20g of bromosafrole to get a 5-6 times molar excess.
All of these posts seem to contradict themselves thus causing jaws's confusion of the term molar excess.
It is because of this confusion that jaws has decided to just use 300-400g of ammonium chloride to be safe, but he would like to better understand this so he is not wasting chems. (especially when he does this rxn with methlylamine)
THE BEST WAY TO AVOID BEEING STUNG IS TO BEE A BEE YOURSELF
(Chief Bee)
12-11-02 18:10
No 388598
Use the molecular weight calculator at https://www.the-hive.ws/forum/pt.pl?Cat=
Ammonium chloride is NH4Cl, and the calculator will tell you that one mole weighs 53.49g.
Bromosafrole is C10H11O2Br and hence weighs 243.1 g/mole.
So, to use a 10x molar excess, you should use 534.9 grams of NH4Cl for every 243.1g of bromosafrole (assuming that 100% of the NH4Cl will end up in the alcohol, which is not true in practice). The 10x figure is good for methylamine, but as NH4Cl is so cheap, if I were to perform the reaction you are working on, I would use about 20-25x molar excess of NH4Cl. How much that is in grams is left as an exercise to the reader
