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Frlt fr att jag skriver i en sdan gammal trd men om ngon dr ute r intresserad i att gra mdma s skriv grna en trd om hur man gr det. Har hrt att det ska vara svrt, jag kan inte mycket sjlv om tillverkning av kemiska droger men funderar p om jag skulle kunna ge mig fan p att lra mig det.
Om ngon skulle pluggat kemi och rent tekniskt sett r kapabel till att tillverka mdma s skriv till mig fr jag r intresserad i att lra mig.
Det r jtte ltt och vem som helst kan gra det i kket s lnge du har en Elvisp och en stor kastrull.
Bara fljd det hr receptet fr 3,5 kg MDMA :
General
Reactions were performed using commercially available raw materials and solvents. Unless otherwise stated, all commercially obtained reagents were qualified prior to use and then used as received. Reactions were conducted in a 50 L reaction vessel. The small-scale production of the Grignard reagent, used to initiate the bulk reaction, was conducted in a 2 L reactor fitted with a reflux condenser. A Huber Unistat was used for temperature control and logging. In-process analysis was conducted by HPLC, with supplemental 1H NMR analysis used to quantify residual solvent content during evaporation steps. A wiped-film evaporator was used for distillation. All processes were conducted under nitrogen (target: <5% O2). Residual solvent testing was performed on an Agilent J&W DB-624 HRGC column (60 m 0.32 mm, 1.80 μm film thickness).
Stage 1─Synthesis of 1-(3,4-Methylenedioxyphenyl)-2-propanol
Grignard Formation
Into a 2 L vessel was charged 16.6 g of magnesium turnings (0.68 mol, 1.1 equiv), followed by 500 mL of THF (181 ppm H2O by KF titration) at 20 C. Stirring was initiated after the introduction of THF, and the vessel was heated to a gentle reflux. To the vessel was then charged 125 g of 5-bromo-1,3-benzodioxole (0.62 mol, 1 equivalent chemical purity >98.70% by HPLC) in two unequal portions. The first portion weighed 6.3 g and was stirred for 12 h at a gentle reflux until an exotherm was observed. Following this initiation step, the remaining 118.4 g was added, dropwise, to the reaction vessel, and the resultant Grignard solution was stirred at reflux for 40 min and then cooled to 25 C.
Into a separate 50 L reaction vessel was charged 1.06 kg of magnesium turnings (44 mol; 1.1 equiv) and 32 L of THF. The suspension was stirred and then heated to a gentle reflux. To the reaction vessel was then added 400.0 g of 5-bromo-1,3-benxodioxole (2.0 mol), followed by 400 mL of the small-batch Grignard solution described above. Reflux was maintained. After 5 min, a significant increase in the reflux rate was observed in the glass condenser, indicating initiation. While maintaining reflux, 7.6 kg of 5-bromo-1,3-benxodioxole (38 mol) was then added to the reaction vessel, using a dropping funnel, and the batch was stirred at a gentle reflux for 40 min.
Addition to Propylene Oxide
The bulk Grignard solution was cooled to 10 C, and 128.8 g of copper iodide (1.5 mol, 0.4 equiv) was added to the 50 L vessel. A solution of 2.5 L ()-propylene oxide (37 mol, 0.93 equiv) in 2.5 L of THF was then added to the reaction vessel while maintaining the temperature at 010 C. The container and dropping funnel were rinsed with an additional 800 mL of THF, which was then added to the 50 L reaction vessel. The batch was stirred for 40 min at 520 C, forming a dark brown solution and a crystalline suspension. Completion analysis performed by HPLC confirmed the reaction end point (0.30% 5-bromo-1,3-benzodioxole; target limit was ≤1%).
The batch was then divided into two 20.4 L portions for workup. For each portion, 5.45 L of a 10% (w/w) sodium chloride solution, followed by 1.37 L of acetic acid, was added to the 50 L reaction vessel while maintaining the temperature at 1025 C. The half-batch portion was then transferred from carboy into the reaction vessel while ensuring that the temperature remained below 40 C. Following this addition, the half-batch portion was stirred at 3040 C for 45 min; then, the pH was adjusted to <5 by sequential addition of three 200 mL of aliquots of acetic acid. The batch was allowed to settle, and the aqueous layer was removed. 8.2 L of n-heptane were then charged into the 50 L reaction vessel, followed by an additional 8 L of the sodium chloride solution. The batch was stirred and allowed to settle, and the aqueous layer was again removed. The dark brown organic layer was filtered over a vacuum, using a plate filter with a 11 μm filter mesh. Following workup, the two half-batches were combined, and the solvent was removed in a 20 L rotatory evaporator. The crude yield was 7442.7 g and analysis by 1H NMR revealed 2.5% residual THF (n-heptane not detected; target limit is ≤10% total amount of both solvents).
The crude product was charged with 1488.5 g of PEG400 (0.2 equiv w/w) and mixed to ensure homogeneity. This mixture was then distilled at 150185 C and 0.11.5 mbar, using a wiped-film evaporator. Two passes yielded 6293.2 g of a pale yellow oil (94.2% yield; 96.44% area, 89.78% w/w by HPLC).
Stage 2─Oxidation to 1-(3,4-Methylenedioxyphenyl)-propan-2-one
A 50 L reaction vessel was charged with 2760.1 g of crude 1-(3,4-methylenedioxyphenyl)-2-propanol from Stage 1 (88.56% w/w by HPLC assay; active charge is 2444.3 g, 13.6 mol, 1 equivalent) and 9780 mL of dichloromethane at 1025 C. Stirring was initiated, and 178.5 g of potassium bromide was added, followed by 233.2 g of TEMPO (0.11 equiv). The batch was cooled to 0 C, and 7280 mL (60%) of a solution of sodium hydrogen carbonate (0.25 equiv) in 12120 mL of bleach (1.6 equiv, diluted to 12.5% w/v) was added, dropwise, while stirring efficiently and maintaining the temperature at −10 to 10 C. A 1 mL of sample was then removed, for analysis by HPLC, and four additional 610 mL (5%) of aliquots of the NaHCO3/bleach solution were then added, dropwise, to the reaction vessel. A sample was collected after each addition, and HPLC analysis was used to monitor the reaction progress. After the fourth aliquot was added, 1.61% of Stage 1 starting material remained (target limit is ≤5%). Stirring was halted, and the layers were allowed to settle. The layers were separated, and the organic layer was returned to the 50 L vessel.
For workup, the organic layer was cooled to 0 C, and 4890 mL of a 12% (w/w) solution of aqueous sodium hydrosulfite was added while maintaining the temperature at 010 C. The reaction mixture was then warmed to 19.5 C and stirred for 15 min. The layers were separated, and the organic layer was returned to the 50 L reaction vessel. Then, 4900 mL of freshly prepared 0.5 M aqueous NaOH was added, and the reaction mixture was stirred for 15 min. The layers were separated, and the brown organic layer was returned to the 50 L reaction vessel. To this were added 4900 mL of 11% (w/w) aqueous NaCl, followed by 98 mL of concentrated HCl 36% w/w aqueous solution. After stirring for 15 min at 18.5 C, the layers were separated, and the organic layer was returned to the reaction vessel. Two more washes─the first with another 4900 mL of the 11% NaCl solution, the second with 4900 mL of a saturated NaCl solution─were completed, following the same procedure. The organic layer was filtered over a Buchner funnel fitted with a filter cloth rinsing with 500 mL of DCM and then transferred to a 20 L rotatory evaporator. The solvent was removed under vacuum, yielding 2442.1 g of a yellow-to-brown oil (101.0% crude yield; 94.52% peak area, 89.80 w/w by HPLC).
Stage 3─Reductive Amination to MDMAHCl
Next, 2963.9 g of crude 1-(3,4-methylenedioxyphenyl)-propan-2-one from Step 2 (13.7 mol, 81.26% w/w by HPLC) was added to a 50 L reaction vessel with 31170 mL of methanol (Kimia, confirmed by FT-IR), and the temperature was lowered to 5 C. Then, 3520 mL of 40% (w/w) aqueous methylamine (102 mol, 7.5 equiv) was added, dropwise, and the batch was then cooled to −10 C. To the reaction vessel was added 40.4 g of NaOH (1 mol) and 286.4 g of NaBH4 (7.6 mol, 0.5 equiv) in 630 mL of purified water, over the course of 120 min. The clear brown solution was then warmed to 3.9 C and stirred for 25 min. A sample was removed and submitted for completion analysis by HPLC; the peak area for the product was 81.04%, and the starting material was undetected, which met the completion threshold of ≤1%. Then, 9640 mL of purified water was added to the reaction vessel, portionwise, while maintaining the temperature at 010 C. The mixture was transferred to a 20 L rotatory evaporator, and methanol was removed, under vacuum. A sample was submitted for analysis, and 1H NMR indicated ≤10% residual methanol, which met the specification.