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Hypothetical Method i might use to Synthesis of MDA/MDMA/MDEA & Methamphetamine
from Protocatechuic aldehyde & Benzaldehyde - By Billbuilds
Methylenation of Catechol aldehyde
Methylene iodide, anhydrous potassium carbonate and copper/bronze oxides were added
to Protocatechuic aldehyde in either DMF or DMSO solvents and reacted under reflux with
stirring. the reaction mixture was transferred to a separatory funnel and washed with 3%
HCl, 3% NaOH & water successively and dehydrated using Na2SO4. the final product was
purified by distillation under vacuum after the removal of solvents.
Preparation of Allylbenzene
[b(trimethylsilyl)ethyl]Lithium was prepared by reaction of HBr and tert-butyllithium at -78
Safrole and Allylbenzene
Addition of pipronal to a solution of b(trimethylsilyl) carbonoim anions in ether at -78
degrees C leads to the formation of trimethylsilyl 3,4 methylene cinnamaldehyde.
Acid treatment of the product with trifluroboro acetic anhydride leads to the dehydration to
an allylsilane and subsequent protonolysis to a the vinyl compound safrole
a three neck round bottom flask is charged with s mixture of palladium chloride, cuprous
chloride in DMF solution with 30% hydrogen peroxide.the allylbenzene is added drop wise
while continuously stirred. the product is separated from the reaction mixture by aqueous
sodium bisulfite solution and cooling the mixture. vacuum filtration separates out the p2p
bisulfite addition product. the filtrate was then transferred to a separatory funnel and
extraction by methylene chloride recovered formed trans-beta-methylstyrene
Allylbenzene and Phenyl-acetone
The trans-beta-methylstyrene formed during the allylbenzene procedure is mixed with
acetone and added drop wise to a solution of hydrogen peroxide in formic acid and the
solution is then refluxed. the solution is neutralized and extracted with methylene chloride .
after evaporation of the methylene chloride the glycol are stirred and heated in a solution
of methanol and dilute sulfuric acid is hydrolyzed for 3.5 hours. the solution is neutralized
with aqueous base and extracted with methylene chloride. the extracted product is added
to the allylbenzene p2p extracts.
A three neck funnel is fitted with a pressure addition funnel, reflux condenser and a
thermometer. To the flask a solution of methylamine and concentrated formic is added.
The temperature is risen to 130 degrees and water is driven off from the reaction mixture.
Then the MD-P2P is added drop wise. The temperature is raised to 150 degrees and held
at reflux for seven hours. Concentrated hydrochloric acid is then added to the solution and
refluxed for an additional eight hours
The solution is treated with sodium hydroxide until alkaline and then the oil produced is
extracted with benzene and washed three times with water and then dried over sodium
sulfate. A concentrated sulfuric acid is added to hydrochloric acid and table salt solution in
a flask with a gas adaptor and a dry stream of HCl gas is bubbled through the the
extracted product to produce the hydrochloride salt which precipitates out..
Substitution ammonia or formamide with ammonium formate to form methylenedioxy
methamphetamine (MDA) or acetamide or ethylamine will form methylenedioxy
To a flask of concentrated formic acid (highest possible concentration). Dry methylamine
gas is bubbled through the3 formic acid forming n-methyl formamide and water. The
concentration of water affects the reaction so using anhydrous materials is essential. dry
methylamine gas can be produced by heating methylamine solution to liberate
methylamine, using a gaseous source of methylamine or the addition of NaOH to
methylamine HCl. The aqueous n-methylformamide is then fractionally distilled under
vacuum to first remove water and then collect anhydrous n-methylformamide.
The phenol-acetone and n-methylformamide are then added to a round bottom flask and
a thermometer attached. the temperature is slowly raised to 105 degrees before the
reaction starts. the heat is leveled off and the reaction allowed to proceed until the reaction
stops and more heat is required. this is continued for 24-35 hours not exceeding 145
degrees. After the solution cools a strong solution of NaOH is added to hydrolyze the nmethylformamide to methylamine and sodium formate. the methylamine gas produced is
piped into fresh formic acid to produce n-methylformamide for the next batch.
The reaction mixture is transferred to a separatory funnel and the aqueous sodium
hydroxide layer is discarded. the methamphetamine formyl amide which floats on the
NaOH layer is then added to a round bottom flask and hydrochloric acid is added and a
reflux condenser applied. A gentle reflux is applied to reduce the methamphetamine formyl
amide to methamphetamine base. after two hours a sodium hydroxide solution is used to
neutralize the HCl reaction mixture. The crude product is extracted three times with
A vacuum distillation apparatus is set up and the toluene extracted under vacuo. The
product is then collected from about 80 -> 140 degrees under full vacuum and added to a
small amount of diethyl ether.. Anhydrous hydrogen chloride gas is then piped into the
flask either from a gas bottle or from a reaction flask of a solution of concentrated
hydrochloric acid and table salt with addition of a slow drop of concentrated sulfuric acid.
The methamphetamine hydrochloride salt then precipitates out. The product is then
collected by vacuum filtration rinsing the crystals with cool solvent to obtain a pure white