Lysergic Acid From Ergot Alkaloids

[Bubbleplate]

In Shulgin's procedure in Tihkal (#26) for making LSD, he starts out by doing an alkaline hydrolysis of Ergotamine Tartrate. After refluxing the alkaloid in the potassium hydroxide solution, dilute H2SO4 is added, which precipitates the Lysergic Acid, and one presumes, some Potassium Sulfate.
He then extracts the Lysergic acid into Ammoniated Ethanol, and then removes the Ethanol under vacumm.

However, he next "dissolves the residual solids in 50 mL of 1% aqueous ammonia, and acidfies the solution as before with 2.5 N H2SO4" to re-precipitated the Lysergic Acid.
My question is, what is the purpose of this second step of dissolving and re-acidfying? Why not just use the Lysergic Acid after evaping off the Ammoniated Ethanol?

[hest]

I'm sure it's the same purpus as rextalisation two times, he get's a cleaner product.
Guess it's not a must to do, but my personal eksp. (not with LSA) is that the GIGO is true (Garbage In Garbage Out)

[Bubbleplate]

by saying that 15% Ammoniated Ethanol should be used to dissolve the Lysergic Acid filter cake. Most other Alkaline Hydrolysis procedures, such as those in Psychedelic Chemistry, and Recreational Drugs, and others, (See Rhodium's Web Site) where liquid Ammonia is added to anhydrous Ethanol, the molar amounts work out to about 5% Ammonia.
My own experience with using Shulgins 15% was that an insoluable purple resin like material formed in the Ethanol, that both interfered with pH readings, and caused reduced yield of Lysergic Acid after second sulfuric acid precipitation. Is it possible that too much Ammonia caused some degradation/breakdown of the Lysergic Acid?

[hest]

Now wee are in the guessing area *gg*
But yes, a higher concentration than nesseserye is usual not to prefere.
And making the hydrolysis is an catalytic reation, so I'm sure that 1 or eaven 0,1% ammonia will doo the trick, unfortunly I have no material to eksperiment on [ wink ]

[Lilienthal]

NH3 is used as a mild and volatile base for alkalinization, not for hydrolysis.

[hest]

Your right
He just use it to form an soluble salt (ammoniumsulphate) Then a 1% solution must bee enough