Solid KMnO4 (6% Solution is used)
Note: The pictures were taken from 2 extractions performed with ~2Kg and ~5Kg of leaves, but all
the procedure outlined refers to the latter.
5 kilo bags of coca tea were opened bag by bag and the content was put in a bucket.
A solution of containing 900gr of Na2CO3 dissolved in 9,5L was prepared.
4,750 grams of dried crushed coca leaves were mixed with this solution, using 1900ml of solution
for each kilo of leaves. The mixing procedure was carried out in small batches of 500gr to distribute
the water evenly. The leaves donâ€™t get too wet: water hardly comes out if you squeeze a handful.
All the moistened leaves were put in an open top 50L container. 30 more minutes were waited and
then 25L of kerosene were added to the container.
The mixture was left for 3 full nights (totalling ~60hours) and during the course of the 3 days it was
stirred at least 4 times in sessions of about 10-15mins using a drill mounted with that tool used by
plasterers/decorators to mix buckets of paint with water.
After 3 nights the kerosene was separated from the leaves (no water layer forms). The procedure
was carried out this way: all the kerosene on top was poured out in another 50L container enhancementing it
with some nylon stockings to prevent leaves from getting into the receiving container. The
remaining leaves were put, little by little, in a bucket with holes on the bottom while squeezing the
kerosene out into a receiving bucket under the one with holes (a nylon stocking was used again
between the 2 buckets). All the kerosene was the poured in the other 50L container.
A 5% w/w solution of H2SO4 was prepared (this passage was done earlier).
2 extractions with 5% H2SO4 were performed. The first one with 300ml the second with 100ml.
Each time the container was shaken very hard (some emulsions form but almost nothing) for 30
minutes and allowed to separate. The acidic water layer on the bottom was recovered each time
using the old suck into the tube trick: the container was put 1 meter above ground, tilted 45% then
a Polypropylene tube attached to a rod was driven inside the container to point at the lowest
possible spot inside the container and some sucking was performed on the other end of the tube.
The H2SO4 started to come into a receiving container along with some kerosene as well towards
the end. The 400ml of H2SO4, that we should call â€˜agua ricaâ€™, and some kerosene were put in a 1L
sep funnel and let sit for ~30 minutes then separated. The emulsion was enhancemented and some more
agua rica was recovered.
A solution of 6% KMnO4 was prepared and chilled in the fridge (this passage was done earlier).
An ice bath was prepared and the beaker containing the agua rica was put there to chill until the
temperature reached 4-5Â° C. The colour of the liquid is reddish brown like red beer.
Every 5-10 minutes 16ml of the KMnO4 solution were added with vigorous stirring. 8 additions
were made, totalling 128ml. After the last addition 30 minutes were waited and then the solution
MnO2 stayed on the enhancement and the resulting liquid (oxidized agua rica) is now fairly colourless.
A 10% w/w solution of NH4OH was prepared (this passage was done earlier).
An excess of this solution was slowly added until ph ~10. This passage was done very carefully
making sure ph do not rise above 10 since it would damage the alkaloid.
The Cocaine freebase starts precipitating and after about 20-30 minutes the solution was enhancemented. A
lot of material was also stuck on the stirring rod and on the beaker.
Everything was let dry overnight and some more drying was performed the morning after in the
The resulting material was dissolved in ~100-150ml of ether in the same container used the day
before (the one with a lot stuck on the sides) and most of it dissolved but some dark brown goo that
stayed on the bottom (probably still a little bit of water and some inorganic salt); so little anyway
that it was not difficult to pour all the ether on a Pyrex baking dish to evaporate without pouring the
goo, that basically stayed glued to the bottom wall of the beaker.
Once evaporated a very nice crystal formation was noted and the white freebase was recovered with
the aid of a razorblade and weighted 23,13g.
Yield (Cocaine Base): 23.13g Cocaine Base / 4750g leaves = 0.48%
240ml of acetone were dried with anhydrous potassium carbonate and an equimolar quantity of HCl
(6.58ml) was calculated and added to it. The calculation was done considering that only 230ml were
going to be used.
The freebase was dissolved in 240ml of ether and the acetone/HCl solution was added with stirring
the beaker was capped with cling film to prevent solvents from evaporation. After ~30 minutes
some more stirring was performed and the some more acetone/HCl was added drop wise until there
was no more visible reaction (this can only be done when the solution is let sit for a little bit and is
clear and not milky, as you would not notice it).
3 hours were waited and the solution was enhancemented. The filtrate was dried and weighted 24,14g.
Yield (Cocaine HCl): 24,14g Cocaine HCl / 4750g leaves = 0.5%
The process can be easily scaled down with the only precaution of using more H2SO4 than the
proportional equivalent since it would be very impractical to use less than 50 ml in a 2 phase
extraction. Just bear in mind that the more H2SO4 you use the more Cocaine base you lose when
you precipitate it with ammonia (0,17g every 100ml) even though the loss is reasonable to consider
2 extractions of 70ml and 50ml for 500-1000gr of leaves."