Hey everyone, I have some questions about this patchwork synthesis for moon rock that I would like some expert feedback and opinions, as well as answers to the following questions below:
a) Is this procedure doable with the procedures and equipment mentioned below, and if so, what are some alternative chems/equipment that can be used to yield a similar or the same results?
b) Below where you see Toluene/Xylene/Methyl tert-butyl ether (TBME), the plan is to use XYLENE, but in the original write up, TBME was used. Will this have any signficant negative effect on the synthesis? Are there special considerations that come with replacing the solvent used in this step? Outside of Toluene/Xylene/TBME, what other solvent could be used?
c) Is the Xylene/solvent used in this step recoverable at all? If so how much can be expected to be recouped (mL)?
d) What exactly is Rochelle Salt used for in the reaction below, and can it be replaced with an analogous salt with similar chemical properties to achieve the same results?
e) This procedure was originally performed under inert conditions (under Nitrogen), what can be modified in the procedure to avoid having to conduct these reactions in an inert atmosphere? Will a dessicant(s) need to be used? If so what/when and where would the drying step take place and are there any special considerations and/or precautions that should be taken when doing this procedure.
f) This write up begins with crude PMK, assuming you start with Ethyl Glycidate, and you perform the necessary conversion to PMK, would that then be considered the "crude PMK" starting material?
Stage 1: Reductive Amination of MDP2P to MDMA-HCl
2963g crude MDP2P was added to a 50 L reaction vessel with 31170 mL of methanol 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. Then, 9640 mL of purified water was added to the reaction vessel, portionwise, while maintaining the temperature at 0–10 °C. The mixture was transferred to a 20 L rotatory evaporator, and methanol was removed, under vacuum.
The crude product was returned to the 50 L reaction vessel and then stirred with 12L Toluene/Xylene/methyl tert-butyl ether (TBME) for 15 min at 18.6 °C. The layers were then separated, and the aqueous layer was washed with an additional 2400 mL of Toluene/Xylene/TBME. The organic layers were then combined in the 50 L reaction vessel; 12 000 mL of 2.0 M HCl was added portionwise, and the mixture was stirred for 20 min at 15–30 °C. At this point, the pH was 1 (target is 1–2), and layers were again separated. The lower, aqueous layer was returned to the 50 L flask, washed with 12000 mL of Toluene/Xylene/TBME and then stirred for 15 min with 6000 mL of 5.4 M aqueous NaOH. Another 12 000 mL of Toluene/Xylene/TBME was then added, along with 1589.6 g of Rochelle Salt/???, and the mixture was stirred for 120 min. The pale brown/orange organic layer was separated from the aqueous layer, and the aqueous layer was washed again with 12 000 mL of Toluene/Xylene/TBME. The organic layers were combined, and the solvent was removed, in batches, with a 20 L rotatory evaporator. Two thousand four hundred milliliters of isopropanol were added to the residue, then removed by a rotatory evaporator. The crude weight of the product (MDMA-free base) was 2524.0 g.
The crude MDMA was then returned to the 50 L flask, along with 20 280 mL of 2-propanol. Stirring was initiated, and 2435 mL 5.4 M HCl in 2-propanol (13.1 mol) was added, dropwise, over 120 min. The mixture was then stirred for an additional 30 min, at room temperature. The white precipitate was captured via vacuum filtration, on a plate filter fitted with a filter cloth. The filter cake was washed twice with 2-propanol (2500 mL) and then dried under vacuum (100 mbar) for 18 h at 57.3 °C. After drying, 2280.4 g of crude MDMA·HCl remained.
Stage 2: Recrystallization of MDMA HCl
To a 50 L reaction vessel was added 4107.3 g of crude MDMA·HCl and 41 000 mL of 2-propanol. The batch temperature was increased to 67.2 °C, while stirring, and the mixture was then stirred for 30 min at 67.2 °C until all of the solids dissolved.
The batch was then transferred through a 1.2 μm in-line filter capsule, using positive pressure, to a clean, 50 L reaction vessel, fitted with a jacket that had been preheated to 66.1 °C. In this new reaction vessel, the batch was cooled to 55.3 °C, over the course of 120 min. The batch was cooled to 15.2 °C at a rate of 3 °C/h and then stirred at this temperature for an additional 10 h.
The white suspension was removed from the mother liquor via vacuum filtration over a filter plate fitted with a filter cloth and then washed with 8220 mL of 2-propanol. The filter cake was transferred to a drying oven and dried under vacuum (140 mbar) for 19 h at 56.6 °C. The collected MDMA·HCl was a white solid weighing 3548.3 g (85.5% yield).
a) Is this procedure doable with the procedures and equipment mentioned below, and if so, what are some alternative chems/equipment that can be used to yield a similar or the same results?
b) Below where you see Toluene/Xylene/Methyl tert-butyl ether (TBME), the plan is to use XYLENE, but in the original write up, TBME was used. Will this have any signficant negative effect on the synthesis? Are there special considerations that come with replacing the solvent used in this step? Outside of Toluene/Xylene/TBME, what other solvent could be used?
c) Is the Xylene/solvent used in this step recoverable at all? If so how much can be expected to be recouped (mL)?
d) What exactly is Rochelle Salt used for in the reaction below, and can it be replaced with an analogous salt with similar chemical properties to achieve the same results?
e) This procedure was originally performed under inert conditions (under Nitrogen), what can be modified in the procedure to avoid having to conduct these reactions in an inert atmosphere? Will a dessicant(s) need to be used? If so what/when and where would the drying step take place and are there any special considerations and/or precautions that should be taken when doing this procedure.
f) This write up begins with crude PMK, assuming you start with Ethyl Glycidate, and you perform the necessary conversion to PMK, would that then be considered the "crude PMK" starting material?
Stage 1: Reductive Amination of MDP2P to MDMA-HCl
2963g crude MDP2P was added to a 50 L reaction vessel with 31170 mL of methanol 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. Then, 9640 mL of purified water was added to the reaction vessel, portionwise, while maintaining the temperature at 0–10 °C. The mixture was transferred to a 20 L rotatory evaporator, and methanol was removed, under vacuum.
The crude product was returned to the 50 L reaction vessel and then stirred with 12L Toluene/Xylene/methyl tert-butyl ether (TBME) for 15 min at 18.6 °C. The layers were then separated, and the aqueous layer was washed with an additional 2400 mL of Toluene/Xylene/TBME. The organic layers were then combined in the 50 L reaction vessel; 12 000 mL of 2.0 M HCl was added portionwise, and the mixture was stirred for 20 min at 15–30 °C. At this point, the pH was 1 (target is 1–2), and layers were again separated. The lower, aqueous layer was returned to the 50 L flask, washed with 12000 mL of Toluene/Xylene/TBME and then stirred for 15 min with 6000 mL of 5.4 M aqueous NaOH. Another 12 000 mL of Toluene/Xylene/TBME was then added, along with 1589.6 g of Rochelle Salt/???, and the mixture was stirred for 120 min. The pale brown/orange organic layer was separated from the aqueous layer, and the aqueous layer was washed again with 12 000 mL of Toluene/Xylene/TBME. The organic layers were combined, and the solvent was removed, in batches, with a 20 L rotatory evaporator. Two thousand four hundred milliliters of isopropanol were added to the residue, then removed by a rotatory evaporator. The crude weight of the product (MDMA-free base) was 2524.0 g.
The crude MDMA was then returned to the 50 L flask, along with 20 280 mL of 2-propanol. Stirring was initiated, and 2435 mL 5.4 M HCl in 2-propanol (13.1 mol) was added, dropwise, over 120 min. The mixture was then stirred for an additional 30 min, at room temperature. The white precipitate was captured via vacuum filtration, on a plate filter fitted with a filter cloth. The filter cake was washed twice with 2-propanol (2500 mL) and then dried under vacuum (100 mbar) for 18 h at 57.3 °C. After drying, 2280.4 g of crude MDMA·HCl remained.
Stage 2: Recrystallization of MDMA HCl
To a 50 L reaction vessel was added 4107.3 g of crude MDMA·HCl and 41 000 mL of 2-propanol. The batch temperature was increased to 67.2 °C, while stirring, and the mixture was then stirred for 30 min at 67.2 °C until all of the solids dissolved.
The batch was then transferred through a 1.2 μm in-line filter capsule, using positive pressure, to a clean, 50 L reaction vessel, fitted with a jacket that had been preheated to 66.1 °C. In this new reaction vessel, the batch was cooled to 55.3 °C, over the course of 120 min. The batch was cooled to 15.2 °C at a rate of 3 °C/h and then stirred at this temperature for an additional 10 h.
The white suspension was removed from the mother liquor via vacuum filtration over a filter plate fitted with a filter cloth and then washed with 8220 mL of 2-propanol. The filter cake was transferred to a drying oven and dried under vacuum (140 mbar) for 19 h at 56.6 °C. The collected MDMA·HCl was a white solid weighing 3548.3 g (85.5% yield).