Author Topic: DMMDA-2 a general approach that works -egotrip  (Read 1025 times)

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dormouse

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DMMDA-2 a general approach that works -egotrip
« on: April 19, 2000, 07:20:00 PM »

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Author  Topic:   DMMDA-2 a general approach that works 
egotrip
NewBee   posted 01-19-2000 08:29 AM          
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dillapiole is brominated w/ dry gas in dmso.
this is a good yielding process. The corresponding cmpd is refluxed in acetone and a molar amount of NaI is added...
This compound, iododillapiole, is very reactive, and when reluxed in denatured alcohol with a slight molar excess of hexamethylenetatramine, turns red, and deposits a crweam colored addition complex that is the stuff. The longer it refluxes the higher the yield, within reason, of course. It will return product with 2-3 hours reflux.
Process the std way ala delepine(HCL,etc)
The red rocklike salt is then processed in the std way.
It really must be distilled at this point, but understand that up till now, it can all be done in an erlenmeyer 500.

This process is sooo general, yet I feel it is very serious chemistry. I dont hear anyone shouting, so I am.


rev drone
Hive Bee   posted 01-19-2000 10:18 AM          
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While normally I'd say this sort of stuff belongs in either the Novel or Chemistry forums due to the lack of heavy-duty theoretical stuff, this certainly sounds interesting anyways. Do you have more detailed notes? Is this thoeretical, or are there some concrete experiments to back this up?
Concentrations, amounts of materials used, reaction times, specific conditions like temperatures and addition rates, -- we need juicy details. It might be serious chemistry, but it looks like it needs some serious fleshing-out. Many thanks for sharing, BTW.

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-the good reverend drone

Ipsa scientia potestas est


 
egotrip
NewBee   posted 01-20-2000 01:47 PM          
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Drone- I have verified this via experiment.
The reaction is so damn general, that I dont really feel the need to specify exact amounts.
re: Concentrations: The actual bromodillapiole was obtained via the dmso/h2so4/NaBr route. 240 ml dmso,18g of 93% h2so4, 56g of NaBr.

However, the HCL generator is aviable alternative, and does generate a dry HBr gas.

Concentrations of NaI- slightly over equimolar.

ditto for the hexamine, which was homemade.

This SHREDS NH3 amination.Really.


Rhodium
Pimp Master   posted 01-21-2000 01:34 PM          
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Write a detailed description anyhow, and I'll include it on my page.
 
rev drone
Hive Bee   posted 01-21-2000 03:57 PM          
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HBr can be generated as a gas using the conventional HCl generator methods? I've heard some things to the contrary (that the HBr generated can decompose into Br2 and H2 if too much heat is present); are you willing to give more information on this? This really would be a wonderful thing.
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-the good reverend drone

Ipsa scientia potestas est