tma-2
- Auteur de la discussion bluegreen
- Date de début
bluegreen
Matrice Périnatale
- Inscrit
- 27/10/08
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- 14
Im just curious why no one responds to this one? Big thread on piper auritum in hydroponics .isnt acorus calamus running along a similar path? the final process looks similar to a laymen.the difference is, if you dont live in Florida this plant is pretty available and hardier.
magickpencil
Alpiniste Kundalini
- Inscrit
- 15/5/08
- Messages
- 674
why don't you just get some fresh Acorus roots?
TMA-2 is not available via the usual route, per-acid oxidation.
Asarone cannot be handled in this fashion. You must utilize the pseudonitrosite reaction to get TMA-2. This is slightly off the beaten path for most, though the chemistry behind the reaction is straightforward and fairly basic, if a little touchy.
http://www.erowid.org/archive/rhodium/c ... /tma2.html
Then, there are other routes which are worth investigating:
http://www.erowid.org/archive/rhodium/c ... ma2np.html
Add to this the fact that there is a bit of a mystery as to whether or not North American varieties of acorus calamus even HAS any beta-asarone in it, and there is your answer.
Physical Properties of Asarone Isomers
Isomer bp12mm d30°/30° nD20° [RL]D
Asarone 167-168°C 1.112 1.5683 62.7
?-Asarone 162-163°C 1.082 1.5552 62.2
Investigate these matters for the definitive answers.
Rhodium is your friend.
Asarone cannot be handled in this fashion. You must utilize the pseudonitrosite reaction to get TMA-2. This is slightly off the beaten path for most, though the chemistry behind the reaction is straightforward and fairly basic, if a little touchy.
http://www.erowid.org/archive/rhodium/c ... /tma2.html
Then, there are other routes which are worth investigating:
http://www.erowid.org/archive/rhodium/c ... ma2np.html
Add to this the fact that there is a bit of a mystery as to whether or not North American varieties of acorus calamus even HAS any beta-asarone in it, and there is your answer.
Physical Properties of Asarone Isomers
Isomer bp12mm d30°/30° nD20° [RL]D
Asarone 167-168°C 1.112 1.5683 62.7
?-Asarone 162-163°C 1.082 1.5552 62.2
Investigate these matters for the definitive answers.
Rhodium is your friend.
ChesireCat
Matrice Périnatale
- Inscrit
- 31/12/08
- Messages
- 6
Chromic wrote a very nice bit detailing the oxidation of Asarone with success using a buffered Peracid. I have been a long time fan of his work and have never had cause to doubt anything he had published. Looks as though the Hatter will have to give this one a go.. Anyway, here is the excerpt from Chromic's work that applies to Asarone.
Oxidation of Propenylbenzenes to P2P's using Peracetic acid
Quick introduction
This method is 100% OTC. It is awesome for a first time chemist who is interested in good yields of their favorite amines and has patience waiting for the peracetic acid to form. It scales very nicely and runs without much hassle. Not one suspect chemical is used.
Preparing the peracetic acid
Make 59.8g of 15% peracetic acid in a clean plastic high-density polyethylene container:
Add 30.2g 35% hydrogen peroxide
Add 29.0g glacial acetic acid
Add 0.6g concentrated sulfuric acid
Swirl the container and allow this to sit for 4-7 days at room temperature before using. Only after the peracetic has aged, continue on.
Running the reaction
Set up a 250ml round bottom flask, sitting in cold-water (no ice) on top of a magnetic stirrer. Now:
Add 100mmol alkene (eg 16.2g isosafrole, see note)
Add 150ml DCM
7.6g NaHCO3 (90mmol)
Drop in a 1" stir bar and start stirring
Slowly pour in the above-prepared 59.8g 15% peracetic acid (118mmol)
This will form a swirling white brew of chemicals in your flask. Fit the flask with a condenser fed with cold water, and allow the reaction to stir for 5 hours.
Extracting the goods
Transfer the mixture to a 500ml sep funnel using a magnet to keep the stir bar in the flask. Add 100ml of 5% NaOH to the sep funnel, shake this vigorously, venting when necessary. Drain off the DCM layer and keep it. Throw out the aqueous layer. Add another 100ml of 5% NaOH. Shake, let settle, and keep the DCM layer. Ensure no aqueous base is in the DCM layer you drained off. Now, distill off the DCM on a water bath and rearrange the oil. The rearrangement is exactly the same as in the rearrangement used in the Oxone method. It is also scaled for 100mmol.
After rearrangement and distillation of the ketone, the typical yields are >60%. (these yields are comparable to the buffered performic in DCM).
Photography chemicals rock. The war is over.
What alkenes can be used?
For those not familiar with what 100mmol alkene is, it is 16.2g isosafrole, 14.8g anethole or 20.8g asarone. This method was tested out with anethole, isosafrole and asarone. The only rearrangement used on the glycol was a 15% H2SO4 rearrangement for just over 2 hours with the presence of methanol as in the Oxone document. All of the ketones were eventually aminated by using methylamine or hydroxylamine to give the intermediate imine or oxime and after Al/Hg reduction to form, respectively, PMA, PMMA, MDMA, MDA, TMMA-2 or TMA-2. Anethole was the easiest to use, isosafrole second and asarone was rather difficult and relatively low yielding. Asarone did produce an exceptional compound, TMA-2, that is highly recommended to those who are looking for something to do after making MDA and MDMA. PMA and PMMA were of some activity but not really worth it for the tasting of the compounds. TMMA-2 was of nearly no activity. I'm positive that isodillapiole and isoparsley apiole could also be used to form their respective amine salts but I haven't had the chance to attempt those reactions although have had the chance to enjoy the pleasurable high of DMMDA-2. I look forward to trying them in the future.
CC
Oxidation of Propenylbenzenes to P2P's using Peracetic acid
Quick introduction
This method is 100% OTC. It is awesome for a first time chemist who is interested in good yields of their favorite amines and has patience waiting for the peracetic acid to form. It scales very nicely and runs without much hassle. Not one suspect chemical is used.
Preparing the peracetic acid
Make 59.8g of 15% peracetic acid in a clean plastic high-density polyethylene container:
Add 30.2g 35% hydrogen peroxide
Add 29.0g glacial acetic acid
Add 0.6g concentrated sulfuric acid
Swirl the container and allow this to sit for 4-7 days at room temperature before using. Only after the peracetic has aged, continue on.
Running the reaction
Set up a 250ml round bottom flask, sitting in cold-water (no ice) on top of a magnetic stirrer. Now:
Add 100mmol alkene (eg 16.2g isosafrole, see note)
Add 150ml DCM
7.6g NaHCO3 (90mmol)
Drop in a 1" stir bar and start stirring
Slowly pour in the above-prepared 59.8g 15% peracetic acid (118mmol)
This will form a swirling white brew of chemicals in your flask. Fit the flask with a condenser fed with cold water, and allow the reaction to stir for 5 hours.
Extracting the goods
Transfer the mixture to a 500ml sep funnel using a magnet to keep the stir bar in the flask. Add 100ml of 5% NaOH to the sep funnel, shake this vigorously, venting when necessary. Drain off the DCM layer and keep it. Throw out the aqueous layer. Add another 100ml of 5% NaOH. Shake, let settle, and keep the DCM layer. Ensure no aqueous base is in the DCM layer you drained off. Now, distill off the DCM on a water bath and rearrange the oil. The rearrangement is exactly the same as in the rearrangement used in the Oxone method. It is also scaled for 100mmol.
After rearrangement and distillation of the ketone, the typical yields are >60%. (these yields are comparable to the buffered performic in DCM).
Photography chemicals rock. The war is over.
What alkenes can be used?
For those not familiar with what 100mmol alkene is, it is 16.2g isosafrole, 14.8g anethole or 20.8g asarone. This method was tested out with anethole, isosafrole and asarone. The only rearrangement used on the glycol was a 15% H2SO4 rearrangement for just over 2 hours with the presence of methanol as in the Oxone document. All of the ketones were eventually aminated by using methylamine or hydroxylamine to give the intermediate imine or oxime and after Al/Hg reduction to form, respectively, PMA, PMMA, MDMA, MDA, TMMA-2 or TMA-2. Anethole was the easiest to use, isosafrole second and asarone was rather difficult and relatively low yielding. Asarone did produce an exceptional compound, TMA-2, that is highly recommended to those who are looking for something to do after making MDA and MDMA. PMA and PMMA were of some activity but not really worth it for the tasting of the compounds. TMMA-2 was of nearly no activity. I'm positive that isodillapiole and isoparsley apiole could also be used to form their respective amine salts but I haven't had the chance to attempt those reactions although have had the chance to enjoy the pleasurable high of DMMDA-2. I look forward to trying them in the future.
CC
HandsCleaN
Matrice Périnatale
- Inscrit
- 19/4/09
- Messages
- 2
Anyone interested should check out the oxone document as well, oxone is cheap pool chemical and is easily made from homade caros acid otherwise....And the claimed yields of epoxide(or diol) are high.....I believe the reason this works so well with asarone is the fact that oxone is a salt, not an acid....But this still leaves the epoxide rearrangement(or pinacol rearrangement) problem as it requires acid...
For higher yields I'd suggest the psuedonitrosite route if you can do it properly, the first few times swim tried it under cheesey reaction conditions and the yields of nitrosite were very poor, under optimal conditions with a real chemistry setup it works....
Most of the calamus on the market is indian calamus oil, which is what you want....Swi-HC distills this under aspirator pressure and a HEAVILY insulated fractioning system, collect never less asarone than 2/3 of the starting weight of the oil...
-Peace
For higher yields I'd suggest the psuedonitrosite route if you can do it properly, the first few times swim tried it under cheesey reaction conditions and the yields of nitrosite were very poor, under optimal conditions with a real chemistry setup it works....
Most of the calamus on the market is indian calamus oil, which is what you want....Swi-HC distills this under aspirator pressure and a HEAVILY insulated fractioning system, collect never less asarone than 2/3 of the starting weight of the oil...
-Peace
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