Written by Chainsaw

LSD from Lysergic Acid Monohydrate

This is, in my opinion, the best of all methods. It was designed to be used to e
xperiment with
different types of amines, so if you would like to substitute diethylamine with
another amine this
would be the best bet. It also gives good yields (50% or better) and is very eas
y. The reference that
gives it (JMC, 16,532(1972)) also gives potency data for many Lysergamides and m
any of their
formulas. The reading is good, interesting, informative, and the method given be
low gives no
useful amount of ISO-LSD, so separation of that product is not necessary.
A slurry of 3.15 g d-lysergic acid monohydrate (monohydrate means dry) and 7.3 g
of diethylamine
(or 0.1 mole of similar amine) in 150 ml of pure chloroform is heated too reflux
. After the lysergic
acid is dissolved (a few min) cool the mixture down to where reflux has stopped
by removing the
heat. Before mixture cools any further 2 ml of phosphorus oxychloride is added a
t such a rate as to
give reflux (about 2 min). After addition, reflux for 4-5 min further until an a
mber-colored solution
result. Cool to room temperature and wash the mixture with 200 ml of 1M ammonium
hydroxide.
The chloroform solution was dried with magnesium sulfate (this would have to be
after separation)
filtered, and concentrated by evaporation in vacuum under a temp of 38 (at no tim
e let the temp
go over 40). The last traces of solvent are removed at 2-5 mm. Dissolved the resi
due in a
minimum amount of methanol and acidify with freshly prepared solution of 20% mal
eate acid in
methanol (not aqueous) to precipitate the LSD in maleate form. Filter the fluffy
white needles,
wash with cold methanol and air dry to get 2.2 g of LSD that requires no further
purification.
Lysergic acid Monohydrate
Dissolve 175 g of KOH in 1,750 ml of water in a flask of 5 liters volume equippe
d with a reflux
condenser and a gas inlet tube. If a stirring device is not required, it should
be removed and the
open neck stoppered. Heat the mixture to 80 under a stream of nitrogen and add 50
0 g of
ergotamine tartrate. Hold the temp at 80 for 2.5 hours with bubbling from the nit
rogen filled gas
inlet tube. Pour the mixture into a 5 gallon polyethylene bucket (mode from the
same material as
in plastic gas cans) filled with about 6 liters of ice. Put the bucket in a cool
ing mixture to cool
below 10C. Neutralize the mixture by adding cold dilute sulfuric acid to a Congo
red end point
(pH 4.2). Lysergic acid and potassium sulfate will be seen to precipitate. Let s
tand for 2-3 hours in
the 5-10 cooling mixture. Filter with vacuum assist, and let vacuum suck as dry a
possible. Break

up the filter cake and put in a 2-liter beaker. Make a solution from 150 ml of l
iquid ammonia and
2.5 liters of very cold dry denatured ethanol and add to the reaction mixture. S
tir for one hour and
filter. Keep the filtrate and treat the filter cake to 1/2 the ammonia ethanol m
ixture as above. This
second extract is filtered and the cake is washed with 250 ml of the ammoniac et
hanol mixture.
Combine the filtrates, and evaporate to total dryness with a strong vacuum and g
ently heating. Do
not heat at too high of a temp. Scrape the product from the vacuum vessel and pu
t into a mortar.
Mix 113 ml of methanol with 38 ml of water, and rinse the rest of the residue fr
om the evaporation
vessel and dump into the mortar with the rest of the product. The slurry in the
mortar is ground up
well and filtered. Wash the filter cake with 1500-ml cold water and use vacuum t
o suck dry for one
hour. Break up the filter cake and dry at 80-85C under a high vacuum to get about
65-75 g of
cream white to gray-white powder. This is Lysergic acid monohydrate. I think tha
t if you dry the
lysergic acid (obtained from the ergot alkaloids by hydrolysis as described earl
ier) it will also work.
This is how you dry lysergic acid: dry under high vacuum at 140-140 C for 2-3 hou
rs
Things you must remember when working with Ergot
Alkaloids, Lysergic acid and LSD
These compounds are very sensitive and even unstable. This means that the follow
ing steps must
be taken to keep from ruining your compound or yield.
1. Always use red or yellow photographic dark room light bulbs during any step o
f LSD
manufacture. Direct sunlight, electric filament, of fluorescent light bulbs (etc
.) will hurt the above
compounds. Dark room bulbs are cheep and are a must.
2. Keep all forms of H2O out of the reaction. Thoroughly dry all the glassware t
o be used. Use a
drying tube filled with anhydrous MgSO4 (calcium chloride reacts with amines in
an unfavorable
way and should be not be used). The drying tube should always be in use even if
water is called for
in the formula. If you are not sure if you should use dry reagents, use dry reag
ents anyway. Also dry
the lysergic acid (as described above) and any other precursor in whatever dryin
g process required
for that compound before use. Dry the finished LSD or even any intermediate alon
g the way after
you have completed the product. Likewise, dry an intermediate that you may have
purchased from
a chemical supplier.
3. Keep oxidizing agents from these items. Even the oxygen in the air can oxidiz
e some of these
compounds. The formula states that during some of the reactions above, an inert
gas (nitrogen)

must be used for an atmosphere inside the reaction vessel. Nitrogen can be obtai
ned in small
bottles (tanks) at a very reasonable fee, without any questions asked. Make sure
you use a
regulator and introduce a slow stream into the vessel by way of a gas inlet tube
or an equivalent.
Always flush the vessel before putting any reagents into it (flush the air out w
ith nitrogen). I would
use a nitrogen atmosphere from the very beginning of the formula to the very end
, even if the
formula did not specify its use. Very few of the above formulas call for a nitro
gen atmosphere
during evaporation, but I feel this may be bad for yield and or potency. LSD has
many doses per
gram, and if you lose 1/4 g because you were too cheep to use three dollars wort
h of nitrogen, you
have lost about 2,000 doses at $5 a dose = $10,000 of LSD wasted. Better safe th
an sorry? Also,
any precursors you make of buy should bee stored in a nitrogen atmosphere, as sh
ould LSD. This
can be done by packing a glass inlet tube into the vessel (just above or a littl
e below the substance)
flushing the air out with a moderate stream of nitrogen then quickly reinstall t
he cap or stopper.
4. Never subject these compounds to excessive heat, or any type of temperature w
armer that the
inside of your refrigerator. Even LSD maleate will decompose in excess heat, so
store in a
refrigerator. Keep evaporation procedures cooled. This will slow the evaporation
process down,
but that is better that losing the product. Some of the above formulas require h
eat for a reaction.
This is OK, but do not exceed the temp stated at any time and never heat longer
than needed.
Also, nitrogen atmospheres are used during heating operation.
Ethylamine, Diethylamine, Triethylamine
These are important intermediates in the synthesis of DMT, LSD and several other
abusable drugs.
This is why they are sometimes difficult to obtain and watched closely by the DE
A. Ethylamine
and trietylamine are not as suspicious as diethylamine because they give weaker
drugs than the
latter. The synthesis to follow will require the knowledge of glass tube sealing
and the dangers of
glass bombs. You may substitute a metal bomb, if it is lined with Pyrex, glass o
r porcelain. I'm not
sure if stainless steel will work here. If you use a large bomb, then it would b
e a good idea to scale
up the amounts of all chemicals involved equimolarly. Making the scale to large
will hurt the yield,
so don't get carried away.
The Chemicals. Ethyl iodide can be purchahaced or made as described in the JCS,
117,1592
(1920). Either way, it must be purified by fractionally distilling, collecting t
he fraction boiling at

71.9-72. Ammonia must be purchased dry and pure or purified and dried according to
the
method recommended by Johnson, J. Chem. Ed., 6,443 (1929), using an excess of so
dium amide.
The reaction is carried out in a sealed Pyrex tube or a suitable replacement. Ca
librate and mark the
tubes, (do not scratch them; use a marker) to a total volume of 20 ml, and dry t
hem by heating in
an oven at 110. Cool and keep them in an atmosphere of dry ammonia (the exclusion
of water of
all types cannot by overstressed in this reaction) until sealed. Into each tube
put 7.5 g of the
dyethel iodine and liquid ammonia is condensed to the 20-ml volume mark by using
a dry ice
acetone bath. The sealed tubes are then transferred to a 0 bath and allowed to st
and at that temp
for 30 min or until they reach that temp. Mix thoroughly by shaking vigorously f
or 1 min. An
exothermic reaction should begin (you will see the bomb contents boil under thei
r own selfgenerated heat) one min after the shaking. Get away from the bombs at this time
(shut them in a
strong cupboard) as bombs sometimes explode. Note: If your are using the glass o
r Pyrex bomb method,
then read a complete book on the subject, so you know the rules to the above and
following procedures as they can
be dangerous.
The bomb tubes are returned to the dry ice-acetone bath. After cooling thusly, t
he tubes are drawn
out to a fine capillary to allow the ammonia to escape, and the entire reaction
mixture is
immediately collected in an excess of dilute HCL acid solution. Evaporate the ac
idic solution to
dryness on a stream bath, desiccate the residue, and extract in a soxhlet extrac
tor for 12 hours
using chloroform as the solvent (dry chloroform) and taking care to exclude all
H2O. Distill off he
chloroform and if separation is not important to you, then you can use the combi
nation of all three
amines in a synthesis calling for any one of the three.
To separate: dissolve the above distillation residue in water. This aqueous solu
tion is agitated in a
separation funnel, with 35 ml of 12 M of NaOH solution and 6 ml of benzenesulfon
yl chloride, to
a total solution volume of 100 ml over a period of 10 min at 0-5. Extract 3 times
with 50-ml
portions of cold ether. Combine the ether extracts and extract them with three 2
5-ml portions of
cold 1M HCL acid solution. The NaOH, the ether, and the HCL acid solutions are t
reated
separately as follows.
The ether extract contains benzenesulfonyl diethylamine, some dibenesulfonyl eth
ylamine and the
excess of benzenesulfonyl chloride. Evaporate the ether, warm the residual oil f
or half an hour,
with 10 ml of 6 M NaOH with enough ethanol to keep the oil in solution (dissolve
d). Cool with a
ice and CaCl mixture, seed by rubbing or scratching a glass rod in the vessel, a
nd with stirring,
dilute slowly with 100 ml of NaCl solution (30 g of NaCl per liter). Allow to st

and for 12-16 hours.

Remove the benzensulfonyl diethylamine by filtration and wash with cold, saturat
ed. (This is not
the same as above NaCl solution). Add the filtrate to the NaOH solution.
Dilute the NaHO solution to 500 ml and evaporate to dryness by heating the vesse
l with a gentle
steam stream and a very low vacuum. The residual product is the ethylamine
The HCL acid solution yielded triethylamine as a picrate when treated with picri
c acid
The Culture and Extraction of Ergot Alkaloids
Make up a culture medium by combining the following ingredients in about 500-ml
of distilled
water in a 2 liter, small-neck flask:
Sucrose-100 g
Chick pea meal-50 g
Calcium nitrate- 1 g
Monopotassium phosphate-0.25 g
Magnesium sulphate-0.25 g
Potassium chloride-0.125
Ferrous sulfate hepahydrate-8.34 mg
Zinc sulfate hepahydrate-3.44 mg
Add water to make up one liter, adjust to pH 4 with ammonia solution and citric
acid. Sterilize by
autoclaving. Inoculate the sterilized medium with Claviceps Purpurea under steri
le conditions,
stopper with sterilized cotton and incubate for two weeks periodically testing a
nd maintaining
pH4. After two weeks a surface culture will be seen on the medium. Large-scale p
roduction of the
fungus can now begin.
Obtain several ordinary 1-gallon jugs. Place a two-hole stopper in the necks of
the jugs. Fit a short
(6-inch) glass tube in one hole, leaving 2 inches above the stopper. Fit a short
rubber tube to this.
Fill a small (500-ml) Erlenmeyer flask with a dilute solution of sodium hypochlo
rite. Fit a long,
glass tube in the other stopper hole. It must reach near the bottom of the jug a
nd have about two
inches showing above the stopper. Attach a rubber tube to the glass tube as shor
t or as long as
desired and fit a short glass tube to the end of the rubber tube. Fill a large,
glass tube (1 inch by 6
inch) with sterile cotton and fit 1-inch hole stoppers in the ends. Fit the smal
l glass tube in the end
of the rubber tube into 1 stopper of the large tube. Fit another small glass tub
e in the other
stopper. A rubber tube is connected to this and attached to a small air pump obt
ained from a
tropical fish supply store. You now have a set-up for pumping air from the pump,
through the
cotton filter, down the long glass tube in the jug, through the solution to the
air space in the top of
the jug, through the short glass tube, down to the bottom of the Erlenmeyer flas
k and up through
the sodium hypochlorate solution into the atmosphere. With this aeration equipme

nt you can
assure a supply of clean air to the Claviceps Purpurea fungus while maintaining
a sterile
atmosphere inside the solution.
Dismantle the aerators. Place all glass tubes, rubber tubes, stoppers and cotton
in a paper bag, seal
tight with wire staples and sterilize in an autoclave.
Fill the 1-gallon jugs 2/3 to 3/4 full with the culture medium and autoclave. Wh
ile these things are
being sterilized, homogenize in a blender the culture already obtained and use t
o inoculate the
media in the gallon jugs. The blender must be sterile. Everything must be steril
e.
Assemble the aerators. Start the pumps. A slow bubbling in each jug will provide
enough oxygen to
the cultures. A single pump can of course be connected to several filters.
Let every thing sit at room temperature (25 degrees c) in a fairly dark place (N
ever expose ergot
alkaloids to bright light as they decompose) for a period of ten days.
After ten days adjust the cultures to 1-% ethanol using 95% ethanol under steril
e conditions.
Maintain growth for another two weeks. After a total of 24 days growth period th
e culture should
be considered mature. Make the culture acidic with tartaric acid and homogenize
in a blender for
one hour. Adjust to pH 9 ammonium hydroxide and extract with benzene or chlorofo
rm/ISObutanol mixture
Extract again with alcoholic tartaric acid and evaporate in a vacuum to dryness.
The dry material is
the salt (i.e., the tartaric acid salt, the tartrate) of the ergot alkaloids, an
d is stored in this form
because the free basic material is too unstable and decomposes.