Clandestine Drug Laboratories

J.W. Gunn, Jr., D.W. Johnson and W.P. Butler
J. Forensic Sci. 15(1), 51-64 (1970)

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During the past three years agents of the Bureau of Narcotics and Dangerous Drugs have seized 95 illicit laboratories. Many others have been seized by state and local police. These laboratories had capabilities of producing drugs worth up to $3,000,000/day on the illicit market. They ranged in size from extensive, well-equipped sophisticated installations to very crude operations carried on in bathrooms, basements, garages, abandoned warehouses — anywhere a manufacturing operation could be established without detection (Figs. 1-3). Quality controls were non-existent, and there was certainly no concern for sanitation, purity or safety of the products produced. Tables I and II indicate the states where the laboratories were located and the types of drugs involved.

Congress recognized, in the Drug Abuse Control Amendments (DACA) of 1965, the need to control the illicit manufacture, compounding, or processing of drepressanty, stimulant and hallucinogenic drugs. Along with these controls, this legislation also prohibits the illegal sale, delivery or other disposition of drugs in these three classes.

When the law was passed in 1965, manufacture and sale were regarded as misdemeanors punishable by up to one year in jail or $1,000 fine, or both. Congress in 1968 through Public Law 90-639, known as the Staggers-Dodd Bill, increased the penalties for trafficking in dangerous drugs to felonies subject to imprisonment up to five years, a fine up to $10,000, or both.

Under the original legislation there was no penalty for possession if the drugs were intended for personal use, for use by members of the household, or for administration to animals belonging to the household. The manner in which the drug was acquired did not effect the legality of its possession.

Under the Staggers-Dodd amendments, the manner in which the drug is acquired does affect the legality of its possession. The amendment permits a person to possess only depressant or stimulant drugs obtained directly from a practitioner who licensed by law to prescribe, or those drugs obtained pursuant to a valid prescription.

Illegal possession for personal use is now punishable as a misdemeanor, with imprisonment of up to one year or a $1,000 fine, or both. Possession with intent to sell is a felony, with penalties equivalent to those for illegal manufacture or distribution.

The law permits persons who use depressant or stimulant drugs in research, teaching, or chemical analysis to possess these drugs or to manufacture them for this purpose. If manufacture is involved, the law requires the person to have registered with the federal government. When possession under these circumstances is encountered, the proof of legal possession rests with the defendant and not with the government as it did before. A problem can arise with clandestine laboratories, when the operation is just getting off the ground and no illegal drug has been produced. The Bureau has been successful in some of these cases by having sufficient intelligence regarding the chemicals and precursors present on the site and the individuals involved in the operations, so that a charge of illegal manufacture of dangerous drugs could be substantiated. Sometimes it is expedient to let the production proceed until an illegal drug has been produced. At that point a charge of failure to register, as well as illegal manufacture and possession, can be made. The Drug Abuse Control Amendments provide for seizure and condemnation of depressant, stimulant, hallucinogenic and counterfeit drugs and any equipment used in the illicit manufacture, compounding or processing. Agents are authorized to make seizures in admiralty libel procedures or by executive seizure prior to the institution of libel proceeding. In the latter instances the property must be brought under the jurisdiction of the court as promptly as possible. Thus, there are ample mechanisms under the law to proceed against violators, their supplies, drugs and equipment.

There has been considerable discussion about how difficult or how easy it is to produce dangerous drugs, particularly hallucinogenic and stimulant drugs, in an illicit laboratory. Some authorities claim that the production of these drugs requires a great deal of skill and experience in organic chemistry, as well as a well-equipped laboratory; however, illicit production of various hallucinogenic and stimulant drugs has been encountered in both crude and sophisticated laboratories, and by amateurs as well as accomplished chemists.

It appears that the illicit production of dangerous drugs has become an intellectual and professional challenge to many individuals associated with their misuse. Some of the more knowledgeable and experienced chemists have achieved clandestine production which approaches commercial scale.

Where does the illegal manufacturer obtain his knowledge? Many of the procedures for the synthesis of controlled drugs are the subject of U.S. patents. Like all patents, these procedures are readily accessible to anyone who desires to obtain them from the Patent Office. Further, during investigation of illicit drug laboratories, individuals were encountered who had made exhaustive searches of the scientific literature for chemical syntheses applicable to the production of hallucinogenic and stimulant drugs. In several of the illicit laboratories raided there were found extensive files of literature on drugs which had been cataloged by type of drug, specific reactions used in the synthesis, and pharmacological action of that particular drug. Copies of extensive review articles on psychotropic drugs were also filed. Many of these clandestine manufacturers are as well aware as any graduate student of chemistry how to use scientific literature as a resource. The great advances made in copying machines have also assisted the illegal operator in obtaining the scientific information that he needs.

For the entrepreneur who is too busy to do his own scientific literature search, many of the methods have been prepared into booklets by other enterprising persons. These booklets sell for $1.50 to $2.00. One such publication has the title “Turn on Book,” subtitled “Synthesis and Extraction of Organic Psychedelics.” There is a question as to whether or not copyrights have been violated in the reprinting of legitimate scientific journal articles in such books. In addition to these books, psychedelic information centers have operated throughout the country which have printed newsletters about the latest drugs, and, in many cases, the “recipes” for their synthesis or manufacture. Much of this material has been “plagiarized” and has been sold separately or compiled into books such as that mentioned above.

In addition to amphetamine and methamphetamine, nearly all of the hallucinogenic drugs on the market today have been produced in illicit laboratories. These include LSD, STP, DMT, DET, mescaline, psilocybin, and phencyclidine, also known as PCP or the Peace Pill. Although synthesis of the tetrahydrocannabinols (THC) which are the active principles of marijuana has been attempted by clandestine laboratories, no laboratory that has been successful has been encountered, nor has any of this drug been found on the street. A number of buys represented as THC have been made, but in most cases the drug has turned out to be phencyclidine. Apparently, the process for making THC is too complicated. It may also be that the raw materials, which are also complex substances, are not readily available or are too difficult to produce in the clandestine lab.

It is not intended to try here to give an exhaustive review of all the syntheses that could be used for the manufacture of the abused drugs; however, some comments on the most commonly encountered syntheses may be of interest.

Lysergic Acid: Lysergic Acid is a must for the production of LSD (lysergic acid diethylamide). Lysergic acids is controlled under the Drug Abuse Control Amendments making its availability limited. Although the total synthesis of d-lysergic acid has been achieved1 the only practical source available to the illicit manufacturer is the hydrolysis of the pharmaceutically important ergot alkaloids, ergotamine and ergonovine. The method of Jacobs, et. al.2, which employs ergotamine tartrate, is frequently used. 100g of ergotamine tartrate will yield approximately 9g of d-lysergic acid monohydrate.

Attempts to manufacture lysergic acid by using a submerged culture method, employing Aspergillus or Claviceps, species paspali or clavatus, also have been encountered. Usually the culture becomes contaminated with Mucor plumbeus or one of the other cosmopolitan organisms.

Lysergic acid diethylamide: Conversion of d-lysergic acid to LSD can be accomplished, theoretically by any common procedures for the formation of amides. The procedure described by Garbrecht3 appears to be most favored. In this method, 9g of d-lysergic acid monohydrate will have a theoretical yield of 10g of the tartrate salts of LSD. The actual yield is about 50% of theoretical.

Other methods are those of Pioch4, Stoll and Hoffman5, and Bernardi and Patelli6.

N,N-Dimethyltryptamine (DMT): DMT, a hallucinogen, which has been called the “Business Man’s Special” because of its short duration of action of one hour of less. It is usually synthesized from indole by the method of Speeter and Anthony7. The final steps in the manufacturing procedure are dependent on how the DMT will be sold. For example, if the DMT is to be placed on a carrier such as tobacco, marijuana or parsley leaves, then the THF solution of DMT is poured over or dropped onto the material to be treated. THF evaporates leaving DMT treated material which can be rolled into cigarettes or sold in packets for use in a pipe.

Pure DMT can be realized by crystallization from the THF solution. A yield of 10-15g may be obtained from 25g of indole.

A substitution of diethylamine for dimethyamine in the synthesis will yield approximately the same amount of DET (diethyltryptamine), a hallucinogenic drug also controlled by the Drug Abuse Control Amendments.

Mescaline: Mescaline may be obtained by the extraction of the alkaloid from the peyote cactus, Lophophora Williamsii, or by chemical synthesis. Both methods have been encountered. The reduction of 3,4,5-trimethoxyphenylacetonitrile with LAH, as described by Tsao8, is a fairly simple procedure which can be accomplished in a crude laboratory. This synthesis will yield approximately 1.2g of mescaline sulfate for 2g of 3,4,5-trimethoxyacetonitrile. When 3,4,5-trimethoxyacetonitrile is not available, mescaline can be synthesized from 3,4,5-trimethoxybenzylchloride or alcohol or the corresponding benzoic acid as described by Tsao. The synthesis, however, becomes longer and more complicated.

Psilocybin and Psilocin: Hoffman9 described the chemical synthesis of psilocybin and psilocin in 1959. During the synthesis of these compounds, DMT is formed first. The further synthesis of psilocybin and psilocin requires considerable additional procedure. This may be the reason why very little of these two hallucinogens has been seen on the illegal market.

Psilocybin can also be produced by biochemical methods using a pure culture of Psilocybe cubensis following the method of Catalfomo10. There have been attempts to follow this route to produce psilocybin but all have been failures.

Amphetamines and Methamphetamines: Of the 95 laboratories seized, 28 were producing stimulant drugs. Methamphetamine, known as “Meth,” “Speed,” or “Crystal” is the most popular product.

Phenylacetone (phenyl-2-propanone) is the primary precursor in the synthesis of amphetamine and methamphetamine. The synthesis of amphetamine have followed the methods of Hartung11,12. In these, hydroxylamine is reacted with phenylacetone, with subsequent catalytic reduction using palladium black as the catalyst with hydrogen under pressure. LAH may be substituted as the reducing agent in these syntheses. By either method, 100g of phenylacetone will yield approximately 130g of amphetamine as the sulfate.

Methamphetamine may be synthesized by reacting phenylacetone with methylamine, with subsequent catalytic reduction with Pd Black and hydrogen under pressure13. LAH has also been substituted in this synthesis as the reducing agent.

Ephedrine reacted with Hydrogen iodide or with HCl acid and Zinc or tinfoil can also produce methamphetamine.

A list of the key chemical reagents needed for the synthesis of the drugs discussed above, as well as for STP and THC, are listed in Table III. A similar list has been furnished to agents of the Bureau to aid them in recognizing materials which have a potential for being used in the manufacture of drugs.

Most of the illicit operations raided by the agents have been those manufacturing the powdered forms of the drugs. One lab had an ampule-filling operation for meth and several had tablet-punching equipment. Most of the tablets from these laboratories were crude productions; however some were expertly made by persons obviously sophisticated in the art of tablet making.

Raiding a clandestine lab can be a dangerous operation. During one raid, an agent had a corrosive material thrown into his face requiring his hospitalization. Many chemicals, including highly flammable solvents and toxic materials, are likely to be present, therefore, it is believed that a chemist should assist the raiding agents. The chemist can be helpful in obtaining the search warrant by describing equipment and chemicals involved, any characteristic or distinctive odors, and possibly he may even identify the drug being produced from these earmarks. After the raid, the chemist can be of help in the collection and preservation of evidence, and can eliminate many exhibits of doubtful value. Because of his knowledge, he can select the necessary items for subsequent lab examination to prove the violation. The Bureau uses chemists in cases involving clandestine labs, and their assistance has been invaluable.

The lab and our forensic chemists are regarded as an arm of enforcement. These specialists can make or break a case. It is essential that the drugs be identified and, in most instances, that a quantitative examination be made. Chemists, trained in modern-day lab instumentation, are absolutely necessary to identify bizarre substances being abused.

Summaries of two cases involving illegal labs may be of interest:

Case 1: A landlord, who took great pride in a home he leased, was irked by his tenant’s failure to maintain the grass in the front of the place. He went to the door to ask that the grass be kept watered but there was no response to his knock. While looking around, he noted an overpowering odor emanating from the house—as if a “dead body” were inside. He called the police who, instead of a corpse, found a clandestine laboratory. Agents of the Bureau were called in on the case, and they found the lab to be a sophisticated facility, with the latest equipment and a wealth of books and reprints from scientific journals. It was operated by a chemist who kept a well-organized lab notebook. The entire water supply of the house was converted to lab use, which accounted fro the failure to water the grass. It took seven truckloads to haul away almost 300 pieces of glassware and equipment. Drugs seized included amphetamines, LSD, mescaline, MDA, STP and several hundred grams of ergotamine tartrate used in the synthesis of lysergic acid. If this quantity of the drug had been converted to LSD it would have produced over $3,000,000 worth of LSD at the going price of $5/trip.

Case 2: Not many months ago, the Bureau learned that a West Coast firm was placing orders with various companies throughout the country for chemical and lab equipment which could be used for manufacturing stimulant drugs. Investigation verified the information and showed that the firm was a supply front for a clandestine meth lab. Interstate surveillance disclosed that the individuals involved flew to various areas of the country in order to pick up supplies. Additional investigation, including aerial surveillance, finally located the lab in a residence in the mountains. Agents on the ground kept the site under observation and witnessed deliveries of chemicals and equipment. Armed with a search warrant and accompanied by the sheriff, a posse raided the lab and arrested four persons. Chemicals, equipment, and about 30lb of manufactured meth, worth nearly a million dollars on the illicit market, was being processed.


Summary

References

  1. Kornfeld, E.C., et al. The Total Synthesis of Lysergic Acid and Ergonovine. J. Am. Chem. Soc., 76, 5256 (1954)
  2. Jacobs, W., and L. Craig. The Ergot Alkaloids. II. The Degradation of Ergotamine with Alkali. Lysergic Acid. J. Biol. Chem., 104, 547 (1934)
  3. Garbrecht, W.L. Synthesis of Amides of Lysergic Acid. J. Org. Chem., 24, 368 (1959)
  4. Pioch, R.P. Preparation of Lysergic Acid Amides. US Patent 2,736,728 assigned to Eli Lilly & Co.
  5. Stoll, A., and A. Hoffman. d-Lysergic Acid-d-1-Hydroxy-2-Butylamide. Helv. Chim. Acta., 26, 944 (1943)
  6. Bernardi, L., and B. Patelli, Process for the Preparation of Lysergic Acid Amides. U.S. Patent 3,141,887 assigned to Societa Farmaceuteci Italia.
  7. Speeter and Anthony. The Action of Oxalyl Chloride on Indoles. A New Approach to Tryptamines. J. Am. Chem. Soc., 76, 6209 (1954)
  8. Tsao, Makepeace U. A New Synthesis of Mescaline, J. Am. Chem. Soc., 73, 5495 (1951)
  9. Hoffman, A. Psilocybin and Psilocin. Two Psychotropically Active Principles of Mexican Hallucinogenic Fungus. Helv. Chim. Acta., 42, 1557 (1959)
  10. Catalfomo, P. The Production of Psilocybin in Submerged Culture by Psilocybe Cubensis. Dissertation Abs. 24, 953, No. 3, (1963)
  11. Hartung, W., and J. Munch. Amino Alcohols. VI. The Preparation and Pharmacodynamic Activity of Four Isomeric Phenylpropylamines. J. Am. Chem. Soc., 53, 1875 (1931)
  12. Hartung, W. Catatlytic Reduction of Nitriles and Oximes. J. Am. Chem. Soc., 50, 3370 (1928)
  13. Ogata, A. Alpha and Beta-Aminoalkyl (Aryl) Benzenes and Their Derivatives. J. Pharm. Soc. Japan., 451, 751 (1919)