Hi,

In Meth process after a reflux of 48 hours rxn with one to condense must one add water and to make heat the rxn during 1 or 2 hours ?

Or it is better to filter water directly ?What is the best way ?

Whoa!! Am I the only one with dificulty understanding wtf atome is asking?

Ask again please, but in english this time.

Wasn't even going to respond to it, since it seemed inchoherent ramblings, but since you bumped it up tot he top.



I concur, please articulate your question a little more intelligible next time Atome.

good

After the reflux what is the best way for stop the reaction ?

1 add hot water and reflux for 1 hours and filter the solution ?

2 add cold water and filter solution ?

I seek only the best way !!!



[This message has been edited by Atome (edited 09-18-2003).]

I think he's asking what to do after the stuff's all done.

Well, usually when your rxn has gone to completion all you'd need to do is add some hot dH2O and filter to remove RP.

However, if you think you're done and your solution isn't pale yellow, you may still have residual I2 left over.

So you may want to reduce the volume of the solution by gently boiling w/o your condensor attatched.

Excess water in the first place will dilute the intended Hydroiodic Acid. Thus making it's reducing potential lower.

quote:

After the reflux what is the best way for stop the reaction ?

So, by adding excess water at the end you essentially stop the reduction process.

After having completed the above procedure. You should have a solution that is free of any particulate matter.

Proceed to, basification of your acidic solution by the slow addition of supersaturated NaOH solution.

Add your preffered NP to extract the freebase. (agitate, agitate, agitate)

Seperate using a seperatory funnel or whatever ghetto method you prefer.

Repeat this extraction, 3 times, the third time you can use a smaller amount of NP.

Next, wash the resulting combined NP extracts with dH2O until the seperated dH20 is no longer registering basic to litmus.

At this point if you are intending to gas your NP to liberate the .hcl salt you may want to considering utilizing a drying agent to remove any excess H2O from the NP containing the amine.

Now, either titrate to produce the amine.hcl in solution, seperate then evap to yield crystals.

Or, gas to produce desired amine.hcl as described in other posts.



Goods Luck