Author Topic: Large scale ET hydrolysis  (Read 3351 times)

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Entheogenea

  • Guest
Large scale ET hydrolysis
« on: December 07, 2003, 04:40:00 PM »
Ok then
A pronoun I know has a fair shitload of ET with no end in sight....

Does anyone out there know of any theoretical limit to the batch size.....i.e. 100g-500g per hydrolysis, maybe more...

This said pronoun ran a batch of 500g into a modified Smith & Timmis and neutralized to pH 5.2 with HCL and freezer treated and yielded quite well on first pass...
This LA from the HCl ppt....yielded via PhosphorousOxy Chloride/DEA superfluffy needles after chromotography over Basic Alumina...etc..

but when the pH was subsequently adjusted to 3.0 with Sulfuric...to harvest more LA....a black coffee brown toffee shit all over the flasks and electrodes etc....

needless to say this pronoun shit bricks....

Pronoun struggled for many months....re-refluxed and tried everthing imaginable....extraction with the Arcemone et. al.  
Isobutanol/Chloroform....then activated carbon...then acidic alumina then reattempts at ppt...all has been unsuccessful for pronoun....ok mostly....pronoun was able to to extract and yes ppt LA via chloroform/ether....yes sounds crazy (would imply freebase LA...never heard of it?)but it worked limited like and yielded good LSD....some xals but the rest amber...

...then extraction attempts via Amberlite IR120 H+ cation exchange resins were attempted and some grey LA sponto xald 
(Xal=crystal) this was ran thru successful...but the 100 plus grams are still lost in Solution....

I do assume by post reading that Kreiselmeier was working with same Ergot product as his was running the same hampster wheel...


Any ideas....may pronoun have just got pronoun's ass kicked by being so fuqn cocky and running to large a batch?

Pronoun is now running 50's on three setups at a time....

Word?

let there be light....


Rhodium

  • Guest
advice
« Reply #1 on: December 07, 2003, 04:46:00 PM »
I think that Mr. Pronoun should run far smaller batches using such a valuable precursor until he has perfected his technique.

Entheogenea

  • Guest
Mr Pronoun Agrees
« Reply #2 on: December 07, 2003, 04:55:00 PM »
Yeah thats an all and good suggestion and one pronoun has Heeded....however....heard of any limits?

I had one guy say he has ran up to 250 but with superclean ET

I heard another say up to 1kg

But then the nicergoline manufacturers must process it on the 10-50kg batch as they are making 10000kg a year of LA

ERGOT the genus claviceps
Harwood Acedemic Publishers
Medicinal and Aromatic Plants - Industrial Profiles
ISBN 90-5702-375X
1999


Rhodium

  • Guest
scale & GIGO
« Reply #3 on: December 07, 2003, 05:03:00 PM »
I think that there is no defined limit to the possible scale, just that the larger the scale, the more careful you need to be to avoid "hot spots" when it comes to temperature, as well as base or acid concentration gradients. Add all reagents dropwise, and with excellent stirring.

Naturally, with a sensitive synthesis like this one, you always should use "superclean" reagents, as any garbage put into a reaction always multiplies to give even more garbage out.

Entheogenea

  • Guest
GIGO
« Reply #4 on: December 07, 2003, 05:09:00 PM »
Yes the GIGO rule applies....

Pronoun has seen various grades of ET....from bone white to tan....

This was tan and the melting point on this batch was a few points low as well..

this shit was only 4 months old but yes had by necessity been thru many package xray machines and such....

now consideration of the method of freebase extraction and then hydrolysis has been on the plate for some time cuz it would eliminate possibility of tartrate from entering the ions in solution equation...

the 50s work to give 13-18g a shot so pronoun is sticking with it until bravery returns...