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3 Synthesis of Methamphetamine: The Clandestine Operation of Choice

3 Synthesis of Methamphetamine: The Clandestine Operation of Choice

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250



18



Clandestine Operations: Synthetic Methods, Hazards, and Safety



Fig. 18.10 The regulation of

common household items is

impossible by anyone’s

standards. Ordinary cookware,

glass containers, and household

products are effectively used to

produce illicit

methamphetamine.



reduce the hydroxyl group on pseudoephedrine. In the process, small pieces of lithium or sodium metal are mixed with pseudoephedrine, and ammonia is slowly added with consistent and vigorous stirring. This part of the process is exothermic and

potentially hazardous. Methamphetamine is subsequently extracted from the mixture using organic solvents. HCl gas is bubbled

through the organic extract to precipitate a usable form of methamphetamine.

HO

NH

CH3

Pseudoephedrine



Structure 18.10



Ammonia



HCl gas



H

N



CH3

Li or Na

reduction



CH3



CH3

d-Methamphetamine



18.3



Synthesis of Methamphetamine: The Clandestine Operation of Choice



251



Fig. 18.11 Hydrogen gas is

stored in metal containers

resembling propane tanks (left).

The gas is used in the last step of

illicit methamphetamine

production. Large Erlenmeyer

flasks are usually found at

clandestine crime scenes (right).



The cold method is preferred by clandestine operators in rural areas of the United States because ammonia is readily available in most fertilizers (Fig. 18.11).



18.3.2



Hot Method



In the hot method, also known as the catalytic reduction of ephedrine/pseudoephedrine, a metal catalyst provides a surface for

the reduction of the hydroxyl (OH) group on ephedrine/pseudoephedrine. There are two common methods for accomplishing

reduction. The first uses palladium (Pd) or platinum (Pt) on activated charcoal (carbon) as the metal catalyst and hydrogen

gas as the reducing agent. The second uses red phosphorus (Red P) as the metal catalyst and hydroiodic acid (HI, strong acid)

as the reducing agent. This is the preferred method used in the United States and is generally known as the red phosphorus–

hydroiodic method (Red-P/HI) (Fig. 18.12).



HO

NH



Pt/Pd/C

CH3

H2 gas



CH3



HO



CH3

Pseudoephedrine



Structure 18.11



CH3



CH3



d-Methamphetamine



Pseudoephedrine



NH



H

N



Red-P, HI



H

N



CH3

heat

reduction



CH3



d-Methamphetamine



CH3



252



18



Clandestine Operations: Synthetic Methods, Hazards, and Safety



Fig. 18.12 Hot method of methamphetamine synthesis.



The Federal Government has passed strict laws regulating the sale and possession of pseudoephedrine-containing tablets.

As a result, clandestine operators are using precursors in ephedra to evade these regulations. When ephedra is used, regardless of the method, a mixture of products is formed.



HO



HO

NH



NH



CH3



CH3

Pseudoephedrine



Ephedrine

Hot or

Cold

method



H

N



CH3



CH3

d-Methamphetamine

(major product)



Structure 18.12



CH3



CH3



NH2

CH3

Amphetamine

(minor product)



CH3

N



CH3



CH3

N,N-dimethylamphetamine

(minor product)



18.6



18.4



Role of the Forensic Chemist at Clandestine Lab Sites



253



Potential Hazards Associated with Clandestine Operations



Clandestine operations vary from site to site; some are small, while others may be large. They may be conducted in a garage,

a backyard, or at remote locations. Regardless of site size or location, all are hazardous to operators, the environment, and

law-enforcement-response teams.

Many clandestine operators are unaware of the potential hazards associated with illicit-drug manufacturing. Their lack of

scientific knowledge is inherently dangerous to themselves, their households, their neighbors, and the environment.

All clandestine lab sites are potentially hazardous due to the necessary presence of various organic solvents, corrosive acids

and bases, and sources of heat or flames. A list of common hazards is below.

1. Chemical reactivity hazard: Clandestine operations require the use of acids and bases, which are both corrosive and caustic. Acid–base reactions are very rapid and, in some cases, extremely violent. They are usually handled improperly and

stored carelessly at clandestine sites, which increases the risk associated with these chemicals.

2. Fire hazard: Many chemicals used in clandestine operations, such as denatured alcohol, charcoal lighter fluid, and

Coleman fuel, are easily ignited and have caused damage to both property and operators.

3. Explosive hazard: Chemical reactions conducted near open flames are extremely dangerous. Many clandestine operations

have been discovered because the operator produced an explosion that destroyed the lab.

4. Exposure hazard: Volatile organic chemicals and HCl gas are frequently used in clandestine operations. Fumes from these

known carcinogens are often present in the facility and surrounding areas. Clandestine operators, their family members,

their associates, and anyone in the immediate area are routinely exposed to these hazardous vapors. Phosphene and phosgene are two deadly gases liberated at various stages of methamphetamine production. They have claimed the lives of

several unsuspecting operators.



18.5



Safety Considerations



Clandestine investigation is the responsibility of specialized, highly trained response teams. Members wear maximum safety gear

upon initial entry and, after assessing the hazard, wear appropriate safety gear while processing the scene (Fig. 18.13).



18.6



Role of the Forensic Chemist at Clandestine Lab Sites



The responsibilities of forensic chemists at clandestine-laboratory crime scenes are outlined below. In addition, they may

also have specific, agency-related assignments.



Fig. 18.13 Clandestine

laboratories are extremely

dangerous and often unpredictable. The safety equipment worn

by response team members

varies at different stages of the

investigation. Initial entry (left)

and crime-scene processing

(right).



254



18



18.6.1



Clandestine Operations: Synthetic Methods, Hazards, and Safety



Advisory



The primary responsibility of a forensic chemist at an alleged clandestine site is to determine whether clandestine operations

actually exist. They assess reagents, chemicals, equipment, and glassware to formulate a preliminary opinion. This is critical

in establishing probable cause for law-enforcement action and also important in the arraignment process. When rendering an

opinion, it is vital to establish whether the site is a current manufacturing or processing facility, or one used in the past.

Differentiation between the two is usually based on experience and common sense. For example, the presence of biphasic

liquids or moist filter paper stained with red phosphorous indicates current manufacturing and processing, whereas dry red

phosphorous, empty jars of iodine, and used, but empty glassware, indicates past activity.



18.6.2



Evidence Collection



If the site is determined to be an active facility, environmental-safety measures are implemented for the processing of

evidence. The forensic chemist identifies relevant evidence and appropriate samples are collected for examination. The evidence is documented and sealed at the scene, and a chain of custody is established for each sample. Transportation of the

evidence to the laboratory is policy dependent; some agencies prefer to transport, while others may defer this responsibility

to the forensic chemist.



18.7

1.

2.

3.

4.

5.

6.

7.

8.

9.

10.

11.

12.

13.

14.

15.

16.

17.

18.

19.

20.



Questions



Can you please explain to the jury the method used to manufacture cocaine?

Outline the procedure for the clandestine production of cocaine.

What is the role of propionyl chloride and sodium hydroxide in fentanyl synthesis?

Why must the pH be closely monitored in the production of g-hydroxybutyric acid?

Draw the reaction for the synthesis of g-hydroxybutyric acid.

Describe the procedure for synthesizing heroin to members of the jury.

Briefly describe the role of acid addition in LSD production.

What is the key intermediate in the synthesis of most methylenedioxy compounds?

Why is hydrogen-chloride gas used in methcathinone synthesis?

Explain the term “bucket method” to members of the jury.

Outline the method used to produce PCP in clandestine laboratories.

How is the Grignard reagent produced?

What is the common precursor to DMT?

Describe the events resulting in the use of ephedra by clandestine operators.

Why is methamphetamine the most common drug produced in clandestine labs?

Outline the hot and cold methods used to produce methamphetamine.

List and describe two hazards associated with illegal-drug manufacturing.

Briefly describe the role of a forensic chemist at clandestine-lab sites.

Discuss two ways to differentiate past clandestine sites from active sites.

Why is establishing “probable cause” important to clandestine investigation?



Suggested Reading

Allen, A. C.; Kiser, W. O. Methamphetamine from Ephedrine: Chloroephedrine and Aziridine. J. Forensic Sci. 1987, 32, 953–962.

Augustine, R. L. Toxic Effects of Impurities in Methamphetamine from Cladestine Labs. Present at DEA Conference, New York, 1979.

Baum, R. M. New Variety of Street Drugs Pose Growing Problems. Chem. Eng. News. 1985, 9, 7–16.

Beagle, J. Q. Synthesis and Effects of PCP Analogs. http://www.erowid.org/archive/rhodium/chemistry/pcp/ (accessed October 2009).

Casale, J. F.; Klien, R. F. X. Illicit Production of Cocaine. Forensic Sci. Rev. 1993, 5, 95–107.

Dal Cason, T. A. An Evaluation of the Potential for Clandestine Manufacturing of 3,4-Methylenedioxyamphetamine (MDA) Analogs and

Homologs. J. Forensic Sci. 1970, 35, 675–697.



Suggested Reading



255



Davenport, T. W.; Allen, A. C.; Cantrell, T. S. Synthetic Reductions in Clandestine Amphetamine and Methamphetamine Laboratories: A review.

Forensic Sci. Int. 1989, 42, 183–199.

Dos Res, L. J.; Maes, R. A. Piperazine-Like Compounds: A New Group of Designer Drugs-of-Abuse on the European Market. Forensic Sci. Int.

2001, 121, 47–56.

Henderson, G. et al. Designer Drugs: The California Experience. In Clandestinely Produced Drugs, Analogues, and Precursors. U.S. Department

of Justice, Drug Enforcement Administration: Washington, DC, 1989.

Metsger, L.; Bittner, S. Autocatalytic Oxidation of Ethers with Sodium Bromate. Tetrahedron. 2000, 56, 1905–1910.

Sanguinetti, V. R.; Angelo, A.; Frank, M. R. GHB: A Home Brew. Am. J. Drug Alcohol Ab. 1997, 23, 637–642.

Shulgin, A. Phenethylamines I have Known and Loved: Synthesis of MDMA; MDM; ADAM; Ecstacy; 3,4-Methylenedioxy-N-Methylamphetamine.

http://www.mdma.net/mdma.html (accessed October 2009).

Shulgin, A.T.; Shulgin, A. DMT Synthesis from Indole. http://deoxy.org/dmt-tihkal.htm (accessed October 2009).

Siegfried. Synthesis of Fentanyl. http://www.opioids.com/fentanyl/synthesis.html (accessed October 2009).

Soine, W. H. Clandestine Drug Synthesis: Heroin. Med. Res. Rev. 1986, 6, 41–74.

United Nations. Guidelines for the Import and Export of Drug and Precursor Reference Standards for Use by National Drug Testing Laboratories;

United Nations Publication: New York, 2007.

U. S. Department of Justice, Drug Enforcement Administration. Synthetically Manufactured Drugs of Abuse, Drug Enforcement Administration:

Washington, DC, 1986.



Evidence Identification and Collection



19.1



19



Clandestine Operations: A Forensic Analogy



Clandestine manufacturing of illicit drugs is a multistep synthetic process that can be accurately compared to preparing a

dinner from a cookbook. First, the raw materials listed in the “recipe” are purchased and separately prepared. Next, the

appropriate cookware is gathered and set up. The ingredients are combined and cooked according to the instructions and the

raw materials are processed into the final product. Impurities are often added to illicit drugs as “cutting agents” to increase

the overall amount of product, which has the effect of increasing profit margins for the operator. Ultimately, the final product

is served and consumed.



19.2



Signs of Clandestine Operations



The evidence associated with clandestine operations is highly variable and depends on a number of factors such as site,

method of manufacturing, type of controlled substance, and quantity produced. These must be considered when formulating a preliminary opinion and collecting evidence for examination. For example, wall stains and carpets stains are

photographed and/or collected for examination to prove that clandestine manufacturing was performed (Fig. 19.1).

It is not a crime to possess acids, bases, organic solvents, plastic tubing, coffee grinders, coffee filters, coffee pots, and

pseudoephedrine tablets. However, a clandestine operation is suspected if:

1. Coffee grinders contain a white solid residue.

2. Coffee pots contain acidic, basic, or organic solvents instead of coffee.

3. There is evidence of red phosphorus or white solid binders present (Fig. 19.2).

4. An excessive number of empty pseudoephedrine blister packs are found on site.

5. Plastic tubing is found connected to plastic or glass bottles (Fig. 19.3).

6. Large quantities of Red Devil Lye (NaOH), acetone, charcoal lighter fluid, denatured alcohol, rubbing alcohol, tincture-iodine,

red phosphorous, muriatic acid (HCl), sulfuric acid, iodine crystals, or hypophosphorous acid are found at the scene.

7. Two-phase (biphasic) liquids are present.



Fig. 19.1 Stains are important evidence in clandestine investigation. Specific types and patterns are often used to indicate the presence of active

clandestine manufacturing.

J.I. Khan et al., Basic Principles of Forensic Chemistry, DOI 10.1007/978-1-59745-437-7_19,

© Springer Science+Business Media, LLC 2012



257



258



19



Evidence Identification and Collection



Fig. 19.2 Red phosphorus

and white solid binders are

strong evidence of clandestine

activity. Red phosphorus is

commonly used in methamphetamine production and binders

are common “cutting agents”.



Fig. 19.3 A variety of

clandestine procedures require

gas-generating systems.

Operators typically produce

primitive systems using

common tubing and readily

available glass or plastic

containers.



19.3



Identification of Related Evidence



Differentiating evidence from common household items at clandestine sites is a delicate process requiring great care. This

task is often complicated by the fact that many chemicals used in clandestine manufacturing have legitimate domestic uses.

Although the presence of the individual items listed below does not necessarily indicate illegal activity, their collective presence at an isolated site is usually a compelling argument for illicit drug production.

1. Solvents: Rubbing alcohol, methanol, denatured alcohol, Coleman fuel, charcoal lighter fluid, and acetone (Fig. 19.4).

2. Elements: Iodine crystals, red phosphorus, lithium, or sodium (Fig. 19.5).

3. Precursors: Ephedrine/pseudoephedrine/ephedra plant.

4. Chemicals: Muriatic acid, sulfuric acid, hypophosphorous acid, hydroiodic acid, sodium hydroxide (Red

Devil Lye), sodium chloride (table salt), or ammonia (Fig. 19.6).

5. Miscellaneous items: Coffee filters, plastic tubing, glass jars, gloves, stained cloths, and biphasic liquids.

6. Equipment: Coffee grinders, electric skillets, stoves, electric scales, coffee pots, heating mantles, and household cookware

(Fig. 19.7).

Propane gas tanks are fairly common in most households. However, clandestine operators modify the cylinders for

storage of corrosive agents such as hydrogen chloride gas or ammonia gas. Therefore, the presence of corroded cylinders

could be an indication of a clandestine operation (Fig. 19.8).

The presence of a small quantity of the items listed above with obvious signs of manufacturing and processing is required for

prosecution. However, large quantities are an indication of illegal use even if found without supporting evidence. For example,

a single bottle of denatured alcohol, or a few packs of pseudoephedrine tablets, would be common in most households, but a

10-gallon drum of alcohol, or a large number of empty bottles of pseudoephedrine, is a clear indication of abuse (Fig. 19.9).



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