Isomerization of Safrole

[Chemtrail]

Hi Beeeees

Swim noticed their is little to no discussion about isomerization of Safrole



Professor Buzz makes a mention of an epoxide oxidation in pg. 51 under Amphetamine
but not the step to isosafrole

Uncle Fester mentions quote " Salfole obtained !fom sassafras oil is Ilrst converted to isosafrole (a propenyl benzene). This is done by
putting safrole into a flask, adding some 10% alcoholic KOH, and then warming the mixture up to 243 C for 3 minutes. This isomerization works just fine so long as absolute alcohol is used, and the alcohol is
allowed to distill off. You know that you have gotten isomerization, because the boiling point of safrole
is 233 C. " in Ch. 19 pg. 190


From a disclosed science article , Swim found this + INCLUDED THE NEXT FOLLOWING EPOXIDE ROUTE TO MDP2P
quote
"
2.3.3.2 Isosafrole from safrole (Route B)

Safrole (1.4 g) was dissolved in a 3 M solution made from potassium hydroxide dissolved in 1-butanol (10 mL, 30 mmol). The resulting solution was heated under reflux for three hours and
allowed to cool.
To the solution, hydrochloric acid (10 mL, 1.6 M) solution was added. The
product was extracted with diethyl ether (3 x 40 mL) and washed with water (3 x 40 mL). The organic extracts were dried over anhydrous sodium sulfate, decanted, and the solvent removed
with a rotary evaporator, producing a brown oil.
Route 1B – Yield: 1.2 g. GC-MS: Figure 5-7.
1H NMR (500MHz, CDCl3): Figure A3-12.
Route 2B – Yield: 1.4 g. GC-MS: Figure 5-8.
1H NMR (500MHz, CDCl3): Figure A3-13.
Route 3B – Yield: 1.4 g. GC-MS: Figure 5-9.
1H NMR (500MHz, CDCl3): Figure A3-14.

2.3.3.3 MDP2P from isosafrole (Route B)

A solution of hydrogen peroxide (2.0 mL, 30%, 20 mmol) in formic acid (10 mL, 23.6 M, 240 mol)
was stirred at room temperature for 30 minutes. A solution of isosafrole (800 mg) in acetone (6 mL) was added and stirred at room temperature for 16 hours. The volatile components of the
resulting solution were removed in vacuo, leaving a red residue.

The residue was dissolved in
methanol (10 mL) and sulfuric acid (10 mL, 2.8 M) was added. The resulting solution was heated
under reflux for three hours and allowed to cool. The product was extracted with diethyl ether
(3 x 40 mL) and washed with of water (40 mL) and a saturated sodium bicarbonate solution (40
mL). The ether extracts were dried over anhydrous sodium sulfate, decanted and the solvent
removed with a rotary evaporator, producing a brown oil.
Route 1B – Yield: 540 mg. GC-MS: Figure 5-10.
1H NMR (500MHz, CDCl3): Figure A3-15.
Route 2B – Yield: 570 mg. GC-MS: Figure 5-11.
1H NMR (500MHz, CDCl3): Figure A3-16.
Route 3B – Yield: 770 mg. GC-MS: Figure 5-12.
1H NMR (500MHz, CDCl3): Figure A3-17. "


THUMBS UP STRIKE
Strike in Total Synthesis II makes a GREAT description of the safrole isomerization conversion to isosafrole
*see Precursors under Isosafrole*

Strike mentions reflux safrole with saturated KOH absolute alcohol for 12-24 hours at 120C-140C. 150c
Filtering may take a lot of time
Filter or not add a Liter of water to a 100-200 ml dark brown oil
Separate the bottom isosafrole oil from the emulsion and dark water junk. Extract the emulsion/dark water junk with a Non Polar fuel 2x-3x s . Combine NP fuel+isosafrole.
Distill the isosafrole (243C - 250C)

Strike also mentions another recipe involving 100g safrole , 15g CaO, 1g KOH and reflux to the boiling temperature of safrole (232C) for 15 minutes. Done


On Erowid : https://www.erowid.org/archive/rhodium/chemistry/isomerizafrole.html

There is a stress importance of minimizing the amount of water in the reaction as much possible !

The use of vacuum for a "vacuum reflux" with the condenser at a vertical position is recommended.

*A hive post mentioned to use a vacuum at the beginning and then off vacuum and proceed refluxing ... for those who don't want to wear out the vacuum the whole night *

Eleusis has a good read on the isomerization of Safrole

Eleusis: Safrole Isomerization v1.5

Swim has a bunch of science articles from the hive, vespiary, etc. about the isomerization of Safrole and swim will include them as attachments pictures included soon

Peace

 

[Chemtrail]

*Edit* like to add from

Complete MDMA synthesis from Sassafras oil with Al/Hg

bbgate.com

Look in the Isomerization section

"The person who did this synthese let s call him SWIM poured the 75 ml safrole in the flask.
He added to this 30 ml 96% ethanol and 21,10 g of KOH.
SWIM refluxed it for 3-4 hours on a gentle reflux of 60 *C.
After adding the KOH to the safrole+ethanol, the mixture turned brown.

Filter to rid of the solid KOH (this reference didn't say wether if it took a long time filtering... He gravity filtered...)

Distill 66 ml isosafrole was the yeild"


An excess of KOH (instead of the 1-10% KOH + absolute alcohol) was noticed

 

[mewnmewamine]

I think the reason nobody talks about it is its kinda pointless no?

also using uncle fester as a source lmaoooooooo have a read through eleusis v fester before you do that again lol

 

[Chemtrail]

Swim thinks it's too odd why nobody hasn't posted anything about isomerization of 3,4 methylenedioxyallylbenzene (safrole)

The science method has been quoted as "laborous" and "low yeilding" and time consuming but with palladium chloride as high as $100 a gram , lots of science articles to use as a helpful reference, and the isomerization to isosafrole and the epoxide oxidation to MDP2P the precursors are all OTC and easy, so is the reason

WITHOUT A DOUBT THE WACKER OXIDATION IS THE WAY TO GO WAY HIGHER YEILDS

MDMA gotta be made some how


...Uncle Fester gets a lot of criticism and haters :/ . In making meth (for example Leukert) you are suppose to put that chemical with P2P for a high temp, then hydrolysis, then base it, then NP fuel extraction and HCl gas. And Uncle Fester did write about such in his book. His science procedure seems right..the whole world hates Uncle Fester lol

 

[mewnmewamine]

I theorize that urushibara nickel would work for wacker oxidations
i do have a hydrogenation vessel sitting there all ready to go once i get the funds just dont have the money rn



ill report back msg me in like 4months if i havent.
^w^ :3

 

[mewnmewamine]

Fester doesnt know what vacuums water aspirators can pull thinks its just the vapor pressure totally doesnt account for temp of water.



Claims things are available when they arent doesnt have basic knowledge on these items eg suggesting methylamine can be bought in gas bottles

Claiming you cant use normal hardware grade hcl for making hcl gas (iirc he doesnt even mention you can use phosphoric/h2so4 to make it)

cotton ball drying tubes lmaooo

His p2pol synthesis is trash

Suggesting you should dry your raney nickel

GLASS BOTTLE HYDROGENATION FUCKING BOMB

The whole "secret method" bullshit in the lsd book where he claims propionyl chloride is used to make lsd because its regulated at such small amounts and the only drug thats that potent is lsd (Salvinorin, fentanyl, bentleys and even some phenethylamines like DOM cos thats active at 1mg)

Suggesting you can brominate safrole with hbr (would cleave the md bridge)

Doesnt know stereochem claims he does

90% of the issues with syntheses on the internet relate back to fester if you are good at chem and in the business of buzzing you have had to solve issues that go back to him.

Read his book and come back to me if you seriously believe he is still an accurate source i severely doubt your aptitude

Also stole most of this from eleusis vs fester while eleusis definitely was right and fester oh so wrong he did have the best line XD

"I know a girl who used to be a guy before that offending part was chopped off, and with no chemistry training she set up shop using the benzaldehyde condensation with nitroethane to get phenylacetone, and then the leukart reaction to get meth. She had low yields on the first run, and after that no problems. Is she a better cook than you?"

 

[mewnmewamine]

Also whoop de fucking do he can copy a leuckart from another place not as if he worked out shit himself

That is the equivalent of you saying "burrr they copy and pasted brightstars first time mdma synthesis"

I fucking hate uncle fester

I would stop washing my pussy for a couple weeks

I would then force him to eat my pussy and ask him "smells like methylamine doesnt it? Oh wait you wouldnt fucking know, You were arrested for possession and buying large quantities of ephedrine"

Fuck fester he can eat shit and die

 

[Chemtrail]

I'm sorry if you feel that about Uncle Fester.

He's not a bad guy . He probably doesn't have any bad intentions to want to hurt people.

There's not a lot of info about meth synthesis out there. He's good.

He has a lot more chemistry experience than I do...

Anyways, This thread is for the Isomerization of Safrole

This thread is for isomerizing allylbenzene (safrole, elemicin, apiole, dillapiole, myristicin)

Anethole and asarone are already isomers and thus propenylbenzene

Just distill fennel seed and star ansie oil to get anethole
*Heard PMA (the drug) is dangerous and causes hyperventilating makes people too hot spasam..*READ EROWID TRIP REPORTS OF PMA & PMMA*

Just distill calamus oil to get asarone

*Heard asarone doesn't do well in acidic epoxide oxidations with big reduced small yeilds

 

[Chemtrail]

Mescalanious hive posts, old forums and relative science articles:

Isomerization Problems , Hive Chemistry Discourse

Safrole isomerization efficiency question , Hive Methods Discourse

" KOH isomerization can be done at 120-130c but require about eight hours. Only running it 130c for four hours provides 80ml from 100ml safrole, but is very clean leaving only amber crystals and no tar allowing multiple batchs back to back with the same KOH residue. "

Isosafrole --> MDP2P via performic and HCl with pictures

" Step 1 Safrole isomerisation at atmospheric pressure

I cant be running a vacuum pump all night so this is my way to go:
Set-up for a regular distillation. Place the safrole(purified by simple distillation under vacuum) along with 2-5% KOH under good stirring. I use about 2.5% and it works like a charm. The temp is brought up to around 180 to get rid of all water. 1 hour at that temp is usually fine, I dont really keep track so much. Then the solution is left to stir at around 140-150 overnight. You dont loose any safrole even without a refluxing column at that temperature . The next morning, vacuum is connected to the system and isosafrole distilled. Yields are always 95-98%. The easy part about this isomerisation is that you only have to rig one setup for the whole process. For those who have never prepared isosafrole, there are 2 distinct properties I use to discriminate. First isosafrole has a different smell then safrole, a lot weaker. Take sniff of safrole. Take a sniff of coffee beans. Smell iso. Its different isnt it? Then look at iso under light. It doesnt refract light as much as pure safrole. I even can see it in the receiver flask as it is distilled. Maybe you will end-up with 1% safrole, but it doesnt change a thing for later stages."

isosafrole

"Preparation of Isosafrole

1. 250ml clear yellow sassafras oil is (optionally) fractionally distilled at 145-50°C under ~60mmHg to clear colorless safrole.
2. Vacuum refluxed in a 2L flask (w/o stirring, no boiling stones) with 1.5wt% ground KOH flakes a la Osmium for 6 hours, the mix turns black
3. Distilled and tossed first 15ml back with unprocessed sassafras, collected over 200ml clear colorless isosafrole at 160-62°C under ~60mmHg.
4. Checked isosafrole by bringing to a reflux at atmospheric pressure and saw that the isosafrole boiled at 254°C. Successful conversion!"

10 degree difference? , Hive Methods Discourse

Rhodium 's words
"When using the more common isomerization methods with a very short reflux (15 min at 230-250°C with KOH/CaO) or at a low temperature (4-12h with 2% KOH under vacuum at 120-130°C), only a part of the higher boiling cis-isosafrole overcomes the energy barrier to be converted to the lower boiling trans-isosafrole, and thus the observed boiling point for the isosafrole cis/trans mixture usually lies closer to 253°C than 246-247°C. "

 

[mewnmewamine]

You can swap koh for an equimolar amount of NaOH

 

[Chemtrail]

And you can also swap everclear 95%ethanol with denatured alcohol

Sure the yellow bottle HEET (99+% methanol) or 99% isopropyl alcohol would work, don't see why not

ABSOLUTE ALCOHOL WITH NO WATER WHATSOEVER IS PRIME as a KOH alcoholic solvent


Some recipes don't even include absolute alcohol like as in no solvent

 

[mewnmewamine]

Yes but you suffer greatly in yields if you dont use any solvent.

Basically everything with an md bridge forms weird tars if you take short cuts.