THE PREPARATORY MANUAL OF NARCOTICS VOL 1.

AMPHETAMINES AND DERIVATIVES

FIRST EDITION

THE PREPARATORY MANUAL OF NARCOTICS VOLUME 1 AMPHETAMINES AND DERIVATIVES

A LABORATORY MANUAL

By: Jared B. Ledgard

Organic chemist, Inventor Seattle, Washington USA

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Table of Contents

Table of Contents
SECTION 1: INTRODUCTION A quick lesson in chemistry Part 1: Introduction to chemistry 1. Chemical bonding: Oxidation states 2. Ionic compounds and ionic bonds 3. Covalent compounds and covalent bonds 4. Understanding chemical structures and formulas 5. Chemical reactions 6. Language of chemistry 7. Conversion factors SECTION 2: LABORATORY TUTORIAL Part 2: Laboratory tutorial on techniques and procedures 8. Introduction 9. Lab safety 10. Laboratory equipment 11. Methods of heating 12. Methods of Cooling 13. Extraction 14. Salting Out 15. Recrystallization, product recovery, and filtration 16. Filtration 17. Washing liquids and solids 18. Drying agents and drying liquids 19. Distillation 20. Apparatus design and function SECTION 3: REFERENCE GUIDE Intermediates, Reagents, and Solvents used in section 3 SECTION 4: AMPHETAMINES AND DERIVATIVES Introduction Notes Synthetic reduction note: replacing lithium aluminum hydride A: Tin and hydrochloric acid technique B: Hydrogenation using nickel, palladium, or platinum with or without charcoal carrier C. Reduction of the nitro intermediates with sodium borohydride 0001. 2-Phenyl-3-aminobutane (freebase). 1-methyl-2-phenylpropylamine Procedure A: Preparation of 2-phenyl-3-aminobutane 0001-02. 2-Phenyl-3-aminobutane sulfate Procedure A: Preparation of 2-phenyl-3-aminobutane sulfate 0002. beta-Methylphenylethylamine hydrochloride. 2-phenylpropan-1-amine hydrochloride Procedure A: Preparation of beta-methylphenylethylamine Hydrochloride 0003. beta-Methyl-(o- and p-)methylphenylethylamine hydrochloride (mixed product) Procedure A: Preparation of beta-Methyl-(o- and p-) methylphenylethylamine hydrochloride 0004. beta-Methyl-p-methoxy-phenethylamine hydrochloride Procedure A: Preparation of beta-Methyl-p-methoxyphenethylamine hydrochloride 0005. N-methyl-omega-phenyl-tert-butylamine. N,2-dimethyl-1 -phenylpropan-2-amine; New Ice; Extravagance. Procedure A: Preparation of N-methyl-omega-phenyl-tert-butylamine Preparation of omega-phenyl-tert-butylamine 0006. -o-Methoxyphenyl-n-propylamine hydrochloride. 2(2-methoxyphenyl)propan-1-amine hydrochloride Procedure A: Preparation of -o-Methoxyphenyl-n-propylamine Page 001 Page 001 Page 001 Page 001 Page 002 Page 003 Page 004 Page 006 Page 006 Page 007 Page 009 Page 009 Page 009 Page 009 Page 010 Page 012 Page 014 Page 016 Page 018 Page 018 Page 019 Page 021 Page 022 Page 023 Page 026 Page 031 Page 031 Page 074 Page 074 Page 075 Page 076 Page 076 Page 077 Page 078 Page 078 Page 078 Page 081 Page 081 Page 082 Page 082 Page 084 Page 084 Page 086 Page 086 Page 087 Page 088 Page 091 Page 092 iii

Table of Contents Hydrochloride 0006-02. -o-Methoxyphenyl propylmethylamine hydrochloride. 1-methoxy-2-(1-methylbutyl)benzene hydrochloride Procedure A: Preparation of -o-Methoxyphenyl propylmethylamine Hydrochloride Intermediate-0007. Ephedrine. 2-(methylamino)-1-phenylpropan-1-ol Procedure A: Preparation of ephedrine (DL and L forms) Procedure B: Preparation of ephedrine (predominately the DL form) Intermediate-0007-02. Extraction of L-ephedrine from Ma Huang herb Intermediate-0007-03. Extraction of pseudoephedrine from store bought pseudoephedrine tablets (Sudafed Galpseud, Novafed, Rhinalair, Otrinol, Sinufed, Symptom 2, Afrinol, and other nasal decongestants and/or bronchodilators) Intermediate-0008. Methedrine. 1-Phenyl-2-methyl-amino-ethan-1-ol Procedure A: Preparation of methedrine (DL and L forms) 0009. Methamphetamine hydrochloride. N-methyl-N-(1-methyl-2phenylethyl)amine hydrochloride; speed; ice; crank; Procedure A: Preparation of methamphetamine hydrochloride Procedure B: Preparation of methamphetamine hydrochloride (direct process; iodine process) Procedure C: Preparation of racemic-methamphetamine hydrochloride (ICE) Intermediate-0010. Safrole. 5-allyl-1,3-benzodioxole Procedure A: Extraction of safrole from sassafras oil Procedure B: Synthesis of safrole from catechol Procedure C: Synthesis of safrole from eugenol Intermediate-0011. Piperonylacetone. 3,4-methylenedioxyphenylacetone. 1-(1,3-benzodioxol-5-yl)acetone Procedure A: Synthesis of piperonylacetone Procedure B: Synthesis of piperonylacetone from black pepper 0012. MDA hydrochloride. 1-(1,3-benzodioxol-5-yl)propan-2-amine hydrochloride Procedure A: Preparation of MDA hydrochloride Procedure B: Preparation of MDA hydrochloride directly from safrole Procedure C: Preparation of MDA hydrochloride from bromosafrole using pressure apparatus Procedure D: Preparation of MDA hydrochloride from piperonylacetone using aluminum amalgam Procedure E: Preparation of MDA hydrochloride Procedure F: Preparation of MDA hydrochloride from piperonal 0013. MDMA. Ecstasy. 3,4-Methylenedioxymethamphetamine hydrochloride. 1-(1,3-benzodioxol-5-yl)propan-2-amine hydrochloride Procedure A: Preparation of MDMA Procedure B: Preparation of MDMA from piperonylacetone via amalgated aluminum reduction Procedure C: Preparation of MDMA Procedure D: Preparation of MDMA directly from bromosafrole 0014. MDEA. Eve. N-ethyl-3,4-methylenedioxyphenylisopropylamine hydrochloride. 5-(2-methylpentyl)-1,3-benzodioxole hydrochloride Procedure A: Preparation of MDEA Procedure B: Preparation of MDEA from piperonylacetone via amalgated aluminum reduction Procedure C: Preparation of MDEA Procedure D: Preparation of MDEA directly from bromosafrole 0015. Amphetamine hydrochloride. 1-methyl-2-phenylethylamine hydrochloride Procedure A: Preparation of Amphetamine hydrochloride Procedure B: Preparation of racemic-Amphetamine sulfate Procedure C: Preparation of racemic-Amphetamine hydrochloride from toluene iv

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Table of Contents 0016. CAT. Methcathinone. 2-methyl-1-phenylbutan-1-one hydrochloride Page 155 Procedure A: Preparation of CAT Page 156 Procedure B: Preparation of CAT using potassium permanganate Page 157 0017. LE-25. 2C-D. 2-(2,5-dimethoxy-4-methylphenyl)ethanamine hydrochloride Page 159 Procedure A: Preparation of LE-25 Page 159 0018. DOM. STP. 2,5-dimethoxy-4-methylamphetamine hydrochloride. 1-(2,5-dimethoxy-4-methylphenyl)propan-2-amine Page 162 Procedure A: Preparation of DOM Page 163 Intermediate-0019. 3,4,5-TMB. 3,4,5-Trimethoxybenzaldehyde Page 164 Procedure A: Preparation of 3,4,5-Trimethoxybenzaldehyde from para-cresol Page 165 Procedure B: Preparation of 3,4,5-Trimethoxybenzaldehyde from vanilla extract (food grade) Page 167 Procedure C: Preparation of 3,4,5-Trimethoxybenzaldehyde from Syringaldehyde Page 169 0020. MESCALINE. M-345. 3,4,5-trimethoxyphenethylamine hydrochloride. 2-(3,4,5-trimethoxyphenyl)ethanamine hydrochloride Page 170 Procedure A: Preparation of MESCALINE Page 171 Procedure B: Extraction of MESCALINE from San Pedro or peyote cactus Page 173 Procedure C: Preparation of MESCALINE (cyanide process) Page 174 0021. BOM. Beta-Methoxymescaline hydrochloride. 3,4,5-betatetramethoxyphenethylamine hydrochloride. 2-methoxy-2(3,4,5-trimethoxyphenyl)ethanamine Page 177 Procedure A: Preparation of BOM Page 178 0022. MMDA. 3-Methoxy-4,5-methylenedioxyamphetamine hydrochloride. 1-(7-methoxy-1,3-benzodioxol-5-yl)propan-2-amine hydrochloride Page 179 Procedure A: Preparation of MMDA Page 180 Procedure B: Preparation of racemic-MMDA Page 183 0023. BOH. beta-Methoxy-3,4-methylenedioxyphenethylamine hydrochloride. 2-(1,3-benzodioxol-5-yl)-2-methoxyethanamine Page 186 Procedure A: Preparation of BOH Page 186 Intermediate-0024. Piperonal. 1,3-benzodioxole-5-carbaldehyde Page 188 Procedure A: Preparation of piperonal from protocatechualdehyde via vanillin Page 189 Intermediate-0025. Eugenol. 4-allyl-2-methoxyphenol Page 192 Procedure A: Extraction of eugenol from cloves Page 192 Intermediate-0026. Myristicin. 6-allyl-4-methoxy-1,3-benzodioxole Page 193 Procedure A: Preparation of myristicin from eugenol Page 193 Procedure B: Preparation of myristicin by isolation from nutmeg Page 196 0027. BDB. 2-Amino-1-(3,4-methylenedioxyphenyl)butane hydrochloride. 1-(1,3-benzodioxol-5-yl)butan-2-amine hydrochloride Page 198 Procedure A: Preparation of BDB Page 198 0028. EDEN. 2-Methylamino-1-(3,4-methylenedioxyphenyl)butane hydrochloride. Methyl-J. N-[1-(1,3-benzodioxol-5-ylmethyl)propyl]N-methylamine; MBDB Page 201 Procedure A: Preparation of EDEN Page 202 0029. THIOMESCALINE. 3,4-dimethoxy-5-methylthiophenethylamine hydrochloride monohydrate. 5-[2-(chloroamino)ethyl]-1,2-dimethoxy-3(methylthio)benzene hydrochloride monohydrate Page 203 Procedure A: Preparation of THIOMESCALINE Page 204 0030. TMA. 3,4,5-Trimethoxyamphetamine hydrochloride. 1(3,4,5-trimethoxyphenyl)propan-2-amine hydrochloride Page 207 Procedure A: Preparation of TMA Page 207 0031. THIOESCALINE. Thioethylmescaline. 3-Thiometaescaline. 4,5-Dimethoxy-3-ethylthiophenethylamine hydrochloride. 2-[3(ethylthio)-4,5-dimethoxyphenyl]ethanamine hydrochloride Page 209 Procedure A: Preparation of THIOESCALINE Page 210 0032. 3M. 3M-Amphetamine. 5-Methoxy-4-methyl-2v

Table of Contents methylthioamphetamine hydrochloride. 1-[5-methoxy-4-methyl-2(methylthio)phenyl]propan-2-amine hydrochloride Procedure A: Preparation of 3M 0033. LOPHOPHINE. 3-Methoxy-4,5-methylenephenethylamine hydrochloride. 2-(7-methoxy-1,3-benzodioxol-5-yl)ethanamine hydrochloride Procedure A: Preparation of LOPHOPHINE 0034. IAP. Indanylamphetamine hydrochloride. 1(2,3-dihydro-1H-inden-5-yl)propan-2-amine hydrochloride Procedure A: Preparation of IAP 0035. Methyl MDA. 5-methyl-MDA. 1-(7-methyl-1,3-benzodioxol-5-yl) propan-2-amine Procedure A: Preparation of Methyl MDA 0036. TMA2. 2,4,5-Trimethoxyamphetamine hydrochloride. 1(2,4,5-trimethoxyphenyl)propan-2-amine hydrochloride Procedure A: Preparation of TMA2 0037. ChloroMescaline. 2-Chloromescaline hydrochloride and 2,6-Dichloromescaline hydrochloride (DCM). 2-(2-chloro-3,4,5trimethoxyphenyl)ethanamine hydrochloride and 2-(2,6-dichloro-3,4,5trimethoxyphenyl)ethanamine hydrochloride (DCM) Procedure A: Preparation of chloromescaline hydrochlorides 0038. DMMDA. 2,5-Dimethoxy-3,4-methylenedioxyamphetamine hydrochloride. 1-(4,7-dimethoxy-1,3-benzodioxol-5-yl)propan-2-amine hydrochloride Procedure A: Preparation of DMMDA 0039. NitroMeth. Para-Nitro-phenyl-isopropylmethyl amine hydrochloride. N-methyl-N-[1-methyl-2-(4-nitrophenyl)ethyl]amine hydrochloride Procedure A: Preparation of nitrometh 0040. Chlorometh. Chlorinated Methamphetamine. para-Chlorophenylisopropyl methylamine hydrochloride. N-[2-(4-chlorophenyl)1-methylethyl]-N-methylamine hydrochloride Procedure A: Preparation of chlorometh 0041. BromoMeth. Brominated Methamphetamine. para-Bromophenylisopropyl methylamine hydrobromide. N-[2-(4-bromophenyl)1-methylethyl]-N-methylamine hydrobromide Procedure A: Preparation of bromometh Final Wrap-up References

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