OK bees, please bee gentle. I have perused Shulgin, Zubrick, Rhodium, and Zwitterion. I've even UTFSE. What I am asking is for confirmation that this collection of independent steps could actually result in a pleasant dream.
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Purification of Safrole from Oil
Main Credits: Chromic, baalchemist
Obtain safrole-containing oil. Attempt purification via fractional crystallization. In the absence of satisfactory purification, attempt purification via fractional vacuum distillation. Target purity should be >95%. All supernatants and waste fractions can be recycled to be repurified later.
Isomerization of Safrole to Isosafrole
Main Credits: Chromic
Expected yield: 80-95%
Add KOH(s) (1-2% by weight) to safrole. Reflux for at least 4 hours. Vacuum distill contents to yield isosafrole. Target yield should be >85%. Waste fractions may be recycled with waste fractions from safrole distillation.
Oxone oxidation of Isosafrole to Glycol/Epoxide
Main Credits: Chromic
Expected yield: 60%
Combine 16.2g isosafrole, 200mL OTC MeOH, and 500mL dH2O. Under continuous stirring, add 85.5g OTC Oxone (85% potassium monopersulfate, 15% pH buffer). Let reaction continue, under agitation, for at least 5 hours. Cease agitation, allow solution to separate, and decant. Save the supernatant. Wash sediment with 4x50mL MeOH and combine washes with supernatant. Add enough dH2O to dissolve any remaining precipitate in supernatant. Extract glycol/epoxide from supernatant with 4x60mL DCM washes. Distill DCM from washes to recover DCM and leave a viscous glycol/epoxide oil.
MDP2P via hydrolysis of glycol/epoxide
Main Credits: Chromic
Expected yield: 95%
Combine 15g glycol/epoxide, 25mL MeOH, and 120mL 15% H2SO4(aq). Reflux mixture for 3 hours. Allow mixture to separate. Retain the dense bottom layer, which should be MDP2P. Wash aqueous layer with 3x40mL DCM and combine washes with the (ketone) MDP2P. Wash ketone mixture with 3x80mL 5% NaOH(aq) and discard washes. Distill DCM off for reuse. Add 50mL safflower oil to ketone oil and vacuum distill. Waste fractions may be recycled with other waste ketone fractions.
MDMA from MDP2P via Amination with Al/Hg/MeNO2
Main Credits: Methyl Man, Dr. Drool, Osmium
Expected yield: >78%
Dissolve 500mg Hg in 50mL 3% tincture of iodine. Wait for color to turn from black/brown to clear (may take up to a week!). Set HgI2/MeOH mixture aside. Combine 25g MDP2P and 50mL MeOH. Use another 50mL MeOH to rinse MDP2P from source container and add to MDP2P/MeOH mixture. Put 27.5g balled Al in reflux flask. Assemble reflux still, start agitation, and pour the HgI2/MeOH mixture into flask. When amalgamation loses shiny silver color, add 20mL 99% MeNO2. Then, add MDP2P/MeOh solution portionwise, slow enough to prevent reaction runaway. If amalgamation thickens up to the point of inefficient agitation, add up to 75mL MeOH into flask. After addition is complete, allow mixture to reflux with no external heating for at least 3 hours.
MDMA freebase via extraction from amalgamation
Main Credits: Methyl Man, Dr. Drool, Osmium, lab_bitch
Expected yield: >90%
Continue agitation and add 750mL 5% NaOH(aq) portionwise. Al/Hg sludge should coagulate and allow relatively easy filtration. Vacuum filter the sludge, then follow with with 5x200mL xylene poured over the Al/Hg mass while still on vacuum. This should extract the MDMA freebase. Purify the freebase either by: washing with 4x500mL dH2O, followed by 500mL saturated NaCl(aq); and/or vacuum distilling freebase at approx 160o[/sub]C.
MDMA.HCl from MDMA freebase via gassing
Main Credits: Found via Grub's post, unknown author
Expected yield: >75%
Note: A better HCl generator can be found in Argox's HCl Generation text. (https://www.thevespiary.org/rhodium/Rhodium/chemistry/hclgas.argox.html)
(https://www.thevespiary.org/rhodium/Rhodium/chemistry/hclgas.argox.html)
Fill wash bottle 1/3 full with CaCl2. Add enough HCl(aq) to cover 2/3 of CaCl2. Let sit for 2 minutes. Submerge wash bottle spout in freebase/xylene mix. Squeeze wash bottle slowly to introduce HCl(g) into solution. MDMA.HCl should precipitate from xylene. Continue gassing until there is no further precipitate can be seen. Vacuum filter the xylene/MDMA.HCl mix. Repeat the gassing-filtering process until no more precipitate forms. If crystals are not of desired purity, recrystallize. Otherwise, enjoy.
(Optional) Recrystallization of MDMA.HCl
Main Credits: LaBToP
Combine MDMA.HCl with enough hot 99% IPA to dissolve. Cool the IPA at a controlled rate, bringing the MDMA.HCl out of solution. Vacuum filter the MDMA.HCl crystals, but save the IPA supernatant. Boil away approx. 75% of the IPA and recool the mixture to precipitate most of the remaining MDMA.HCl. Vacuum filter these crystals, combine the MDMA.HCl aliquats, and store in an anhydrous container, perhaps even along with a silica gel (or other dessicant) packet.
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So, master bees, what is the consensus? I throw myself upon your mercy. Thank you for any feedback I receive, good or bad.
*** If this is simply an illusion, does that mean hallucinations are reality? ***
Oh, wonderful. If everyone could research so well before trying to synthesizing something...
Add 50mL safflower oil to ketone oil and vacuum distill.
"Buffer oil" is superstition, and serves no purpose in organic chemistry. The source of the misinformation is Eleusis, interpreting the term "chaser solvent" in Zubrick all wrong.
After reflux flask has cooled, continue agitation and add 3x250mL 5% NaOH(aq).
I have no idea about what you are trying to do here. Why not say "add 750ml 5% NaOH portionwise"?
(Optional) Recrystallization of MDMA.HCl
Very bad chemistry. Recrystallize from 7 times the weight of the MDMA.HCl in acetonitrile, or dissolve in the minimum necessary amount of boiling 99% isopropanol, then dilute with twice the amound of diethyl ether and let cool to 0°C for an hour or two, filter and wash the crystals on the vacuum buchner funnel with dry ether.
Do not use acetone with MDMA for washing, "crashing" or recrystallization. The acetone can condense with the amine, forming an enamine.
You are recycling your solvents, that is excellent. You are overestimating the importance of fractionating your precursors and collecting foreruns for re-processing (unless you are unusually cheap, have a real problems obtaining precursors, or have reason to believe that the step failed.
ClearLight is right, you should distill your MDMA freebase at ~160°C using an aspirator before crystallize the hydrochloride. Your HCl generator will probably work ok, but I think https://www.thevespiary.org/rhodium/Rhodium/chemistry/hclgas.argox.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/hclgas.argox.html)
is better.
That way of performing a Nitromethane/MDP2P reductive methylamination is not reccommended. Instead add the nitromethane first, and when all of it has been reduced to methylamine, then add the MDP2P and continue the reduction.
Suggested reading:
Post 357309 (https://www.thevespiary.org/talk/index.php?topic=6926.msg35730900#msg35730900)
(Osmium: "my preferred way", Chemistry Discourse)
Post 363298 (https://www.thevespiary.org/talk/index.php?topic=9897.msg36329800#msg36329800)
(Osmium: "If your reaction is running so hot that it stinks ...", Methods Discourse)
Oxone oxidation of Isosafrole to Glycol/Epoxide
can this step bee scaled? it says 60% yield...but the next step uses 93% yield weight?! can SWIM make a double batch for this step? or half the next steps ingredients in order to accomodate the yield loss?
this step also doesn't mention the baking soda...if it's used, will that slow the rxn? damage the desired product?
It tastes like burning! :o :P
Do not use acetone with MDMA for washing, "crashing" or recrystallization. The acetone can condense with the amine, forming an enamine
Rhodium: I am curious about this statement because many of the posts that I've gone through for suggestions and procedure do recommend washing finished product with acetone. Mainly I'd like to know if enamine formation is a concern from the point of view of toxicity. Thanks.