meme (Hive Bee)
10-01-01 21:15
No 219103
      Seperation of dmt/5meo  Bookmark   

After an extraction of the crude alkaloids, if SWIM dissolved the freebase in high concentration aqaeous acetic acid, buffered with NaCH3COO, upon subsequent washing with NaOH, with a non-polar layer for extraction, and using a tryptmaine testing kit, would it bee possible to seperate these two alkaloids?

I originally posted this at dmtworld, which is down right now . . .



Today is opposites day.  Everything I say, I mean the opposite.
 
 
 
 
    meme
(Hive Bee)
10-08-01 22:55
No 221814
      Re: Seperation of dmt/5meo  Bookmark   

No one? 



Today is opposites day.  Everything I say, I mean the opposite.
 
 
 
 
    Rhodium
(Chief Bee)
10-08-01 23:32
No 221834
      Re: Seperation of dmt/5meo  Bookmark   

I believe it is only possible by column chromatography (or kugelrohr distillation).
 
 
 
 
    Lilienthal
(Moderator)
10-09-01 00:51
No 221870
      Re: Seperation of dmt/5meo  Bookmark   

Vacuum distillation should work also. Could you explain that strange extraction?
 
 
 
 
    Rhodium
(Chief Bee)
10-09-01 01:48
No 221900
      Re: Seperation of dmt/5meo  Bookmark   

How high vacuum is really needed for tryptamines? At 3 mmHg the bp of DMT is already over 200C (extrapolated with nomograph).
 
 
 
 
    Lilienthal
(Moderator)
10-09-01 02:49
No 221933
      Re: Seperation of dmt/5meo  Bookmark   

You need oil pump vacuum:

Boiling Point 1-2 of 2
80C - 135C  0.03 torr  (1)
160C  0.6 torr  (2)
Ref. 1 2570130; Journal; Corothie; Nakano; PLMEAA; Planta Med.; 17; 1969; 184,186.
Ref. 2 6217095; Journal; Haefelinger, Guenter; Nimtz, Manfred; Horstmann, Volker; Benz, Thomas; ZNBSEN; Z.Naturforsch.B; GE; 54; 3; 1999; 397 - 414.
 
 
 
 
    wandering101
(Hive Bee)
10-09-01 16:58
No 222254
      Re: Seperation of dmt/5meo  Bookmark   

This was basically the only reference I found on the web for kugelrohr distillation (OK, I didn't THAT much time looking)
http://www.jepbol.com/sect1/dist.html (http://www.jepbol.com/sect1/dist.html)
What exactly is "kugelrohr distillation" - this page didn't make much sense to me.
 
 
 
 
    Rhodium
(Chief Bee)
10-09-01 18:52
No 222301
      Re: Seperation of dmt/5meo  Bookmark   

It is a $2500 short-path distillation apparatus for small amounts of thick oils and other high-boiling substances.
 
 
 
 
    Lilienthal
(Moderator)
10-09-01 20:08
No 222328
      Re: Seperation of dmt/5meo  Bookmark   

All you need is an oil pump and several of these glass bulbs of 3 - 4 cm in diameter with connecting joints at their top and their bottom. You can rotate this Kugelrohr manually over a heat source if you use rubber vacuum tube smile
 
 
 
 
    wandering101
(Hive Bee)
10-11-01 15:09
No 223150
      Re: Seperation of dmt/5meo  Bookmark   

Ahh. Many thanks.
I don't see myself building one anytime soon - I don't have much that will require this, but it's always a good thing to know.
Or I'll go find myself a use....
 
 
 
 
    meme
(Hive Bee)
10-17-01 17:56
No 225814
      Re: Seperation of dmt/5meo  Bookmark   

" A sol.n containing acetic acid, CH3COOH, and sodium actetate, NaCH3COO, is an example of this kind of buffer soln. The acidic component is CH3COOH. The basic component is NaCH3COO because the CH3COO- ion is the conjugate base of CH3COOH, The operation of the buffer depends on the equiibrium.

CH3COOH + H2O +---+ H30+ + CH3COO-
(high conc.) (high conc from salt)

When a strong base, such as NaOH, is added to the CH3COOH-NaCH#COO buffer solution, it is consumed by the acidic component CH3COOH. This occurs in the following way. The additional OH- causes the water autoionization reation to proceed to the left.

2H2O +---+ H3O+ + OH-

This uses up some H3O+, causing more CH3COOH to ionize.

CH3COOH + H2O +---+ CH3COO + H3O+ (shifts right)

Because the [CH3COOH] is so high, this can occur to a great extent. The net result is the neurtalization of OH- by CH3COOH.

OH- + CH3COOH -----+ CH3COO- + H2O (~100%)
added base acid weaker base water


"The solution, it turns out, would have to be very high is acetic, but not glacial, as it would need water. Here's some related info.

When we add 0.0010 mol NaOH

We have 1 L of original soln ph increases H3O decreases

Buffer soln +0.008 ph unit 1.2
(0.10 M NaCh3COO +
0.10 M Ch3COOH )


0.10 CH3COOH 0.91 8.1

Pure H2O 5.00 100,000


General Chemestry with Qualitative Analyses 6/e
2000 Harcourt College Pub. Orlando, FL.
**************

Basically, since such small changes in ph are possible using a buffered solution, differing alkaloids can be seperated based on the (minute) differences in ph.

The idea was mentioned in general in Indole Alkaloids, I don't have this around to ref the author or mention, but it was something like " A buffered soln was washed to yeild alkaloids of differing strengths based on their ph"



Today is opposites day.  Everything I say, I mean the opposite.