Reagents Needed:
Kerosene,
Solid Na2CO3,
Distilled H2O,
H2SO4 5%
Solid KMnO4 (6% Solution is used) NH4OH 10%,
HCl 37%,
Acetone,
Diethyl Ether.
Note: The pictures were taken from 2 extractions performed with ~2 Kg and ~5 Kg of leaves, but all the procedure outlined refers to the latter.
Procedure:
5 kilo bags of coca tea were opened bag by bag and the content was put in a bucket.
A solution of containing 900 gr of Na2CO3 dissolved in 9,5L of water was prepared.
4,750 grams of dried crushed coca leaves were mixed with this solution, using 1900 ml of solution for each kilo of leaves. The mixing procedure was carried out in small batches of 500 gr to distribute the water evenly. The leaves don’t get too wet: water hardly comes out if you squeeze a handful.
All the moistened leaves were put in an open-top 50 L container. 30 more minutes were waited, and then 25 L of kerosene were added to the container.
The mixture was left for 3 full nights (totalling ~60 hours) and during the course of the 3 days it was stirred at least 4 times in sessions of about 10-15 mins 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 50 L container, filtering 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 50 L 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 300 ml, the second with 100 ml. 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 400 ml of H2SO4, that we should call ‘agua rica’, and some kerosene were put in a 1L sep. funnel and let sit for ~30 minutes then separated. The emulsion was filtered 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 4-5 °C. The colour of the liquid is reddish brown, like red beer.
Every 5-10 minutes, 16 ml of the KMnO4 solution were added with vigorous stirring. 8 additions were made, totalling 128 ml. After the last addition 30 minutes were weighted and then the solution was filtered.
MnO2 stayed on the filter, 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 filtered. 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 oven.
The resulting material was dissolved in ~100-150 ml 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 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 razor blade and weighted 23,13 g.
Yield (Cocaine Base): 23.13 g Cocaine Base / 4750 g leaves = 0.48%.
240 ml of acetone were dried with anhydrous potassium carbonate and an equimolar quantity of HCl (6.58 ml) was calculated and added to it. The calculation was done considering that only 230 ml were going to be used.
The freebase was dissolved in 240 ml 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 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 and is clear and not milky, as you would not notice it).
3 hours were waited, and the solution was filtered. The filtrate was dried and weighted 24,14 g.
Yield (Cocaine HCl): 24,14 g Cocaine HCl / 4750 g 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 (0,17 g every 100 ml) even though the loss is reasonable to consider 2 extractions of 70 ml and 50 ml for 500-1000 gr of leaves.
Kerosene,
Solid Na2CO3,
Distilled H2O,
H2SO4 5%
Solid KMnO4 (6% Solution is used) NH4OH 10%,
HCl 37%,
Acetone,
Diethyl Ether.
Note: The pictures were taken from 2 extractions performed with ~2 Kg and ~5 Kg of leaves, but all the procedure outlined refers to the latter.
Procedure:
5 kilo bags of coca tea were opened bag by bag and the content was put in a bucket.
A solution of containing 900 gr of Na2CO3 dissolved in 9,5L of water was prepared.
4,750 grams of dried crushed coca leaves were mixed with this solution, using 1900 ml of solution for each kilo of leaves. The mixing procedure was carried out in small batches of 500 gr to distribute the water evenly. The leaves don’t get too wet: water hardly comes out if you squeeze a handful.
All the moistened leaves were put in an open-top 50 L container. 30 more minutes were waited, and then 25 L of kerosene were added to the container.
The mixture was left for 3 full nights (totalling ~60 hours) and during the course of the 3 days it was stirred at least 4 times in sessions of about 10-15 mins 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 50 L container, filtering 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 50 L 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 300 ml, the second with 100 ml. 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 400 ml of H2SO4, that we should call ‘agua rica’, and some kerosene were put in a 1L sep. funnel and let sit for ~30 minutes then separated. The emulsion was filtered 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 4-5 °C. The colour of the liquid is reddish brown, like red beer.
Every 5-10 minutes, 16 ml of the KMnO4 solution were added with vigorous stirring. 8 additions were made, totalling 128 ml. After the last addition 30 minutes were weighted and then the solution was filtered.
MnO2 stayed on the filter, 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 filtered. 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 oven.
The resulting material was dissolved in ~100-150 ml 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 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 razor blade and weighted 23,13 g.
Yield (Cocaine Base): 23.13 g Cocaine Base / 4750 g leaves = 0.48%.
240 ml of acetone were dried with anhydrous potassium carbonate and an equimolar quantity of HCl (6.58 ml) was calculated and added to it. The calculation was done considering that only 230 ml were going to be used.
The freebase was dissolved in 240 ml 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 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 and is clear and not milky, as you would not notice it).
3 hours were waited, and the solution was filtered. The filtrate was dried and weighted 24,14 g.
Yield (Cocaine HCl): 24,14 g Cocaine HCl / 4750 g 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 (0,17 g every 100 ml) even though the loss is reasonable to consider 2 extractions of 70 ml and 50 ml for 500-1000 gr of leaves.
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