A small exchange of experiences with FesterFormula

[Methlaab]

Hi Beeees,


I would be really glad about swim's experiences, especially how the quality of a product produced by the Fester Formula is (electrolytical reduction]

Thx, to all who can help me

[UncleFester]

Here's one...if one switches the electrolyte to dilute HCl to try to avoid that problem with sulfate salts not hydrogenating very well, the chlorine generated at the anode isn't stopped by even two layers of condoms, and leaks right into the product compartment, bleaching it all. Maybe a sacrificial anode would work in HCl.

[Methlaab]

ok thanks for answering...

I would like to know, if you don't think that best results are got by using 10-20% sulfuric acid as anolyte and as catholyte I would prefere to use a solution of hydrochloric acid of less than about 10%. then I would put the nitro...compound to be reduced to into the cathode compartment of my reaction cell. Then I would an courent of about 0.1 to 0.2 ampere per square centimeter let pass through the cell. And while courent passes the temperature of cell is maintained between 50°-100°C....ok thats the non-specific theory

and if you wanna hydrate ephedrine to (+) N-Methyl-beta-phenyl-isopropylamin, then I would use for example 4g of ephedrine HCl disolved in 90ccm actetic acid. To this solution 4,7g of sulfuric acid of 84% and also 1g Palladium are added and hydrated at a temperature of 60°C and 3,5 atü. After 1 mol of H is exhausted the reaction ends. while filtering the catalyste the sulfuric acid is neutralized with dry soda, the actetic acid is distilled of in vaccum and the residuent is after the adding of conzentrated NaOH as long treated with steam untill no amine distilles. the distillate which is neutralized with HCl is evaporeted in vaccum as a result you will get (+)-methyl-beta-phenylisopropylamin in a quantity of 95%. Its meltingpoint is about 166°-168°C after crystallization it melts at 172°C.

[UncleFester]

Rhodium wants me to give links to Patents mentioned, and now is a really good time to start...thing is I went to the FAQ section, spent 5 minutes there(the kids were telling me it's time to go to the ballgame) and all I saw was how to make blinky faces on the post. I'll just wing it and guess from the menu at the post page bottom. Get to

Patent US6399828

, read it and read it again...each time you will learn more from it...heating the ephedrine with acetic and sulfuric is a method they don't like for making ester..but making ester they like a whole lot. Without ester, they get no reduction to meth....I'll comment more later after just heading to the bottom of the page and trying to mark the US Patent. The kids are yelling at me saying the ballgame is going to start as we speak... damn I clicked and double clicked on the Patent button and nothing happened...and the kids are yelling at me...got to go for now...check it out at www.uspto.gov, and type in the number...

[readyeddie]

http://patft.uspto.gov/netacgi/nph-Parser?Sect1=PTO1&Sect2=HITOFF&d=PALL&p=1&u=/netahtml/srchnum.htm&r=1&f=G&l=50&s1=6%2C399%2C828.WKU.&OS=PN/6%2C399%2C828&RS=PN/6%2C399%2C828

[Methlaab]

thank you a lot...I'm going to read the patent and then I will maybe add anymore...

so far

[WizardX]

Have a look at this to make the ephedrine acetate ester.

http://www.orgsyn.org/orgsyn/prep.asp?prep=cv9p0507

  Look at part C.

[UncleFester]

The acetyl chloride would also react with the amine portion of the molecule to make an amide.

[BullwinkleMoose]

A HAlo Ephy by Dwarfer

ORGY QUOTE"
Where is Dwarfer btw.? I have the feeling his microwave chlorination with HCl/Zn should be better explored - I believe he turned more ephedrine to meth in this step than in the following electrolysis. This is more promising than anything else for a quick and dirty one shot-conversion for endusers."

[readyeddie]

What would be the best otc replacment for heptane for crystalizing when making the ester from acetic anhydride.

[Lestat]

Heptane is the only other thing in OTC ether based
easy-starting fluid and is fairly nonvolatile, so the ether can bee CAREFULLY distilled off and saved leaving heptane beehind.

What about using n-hexane instead? freely available as dry cleaning fluid type stuff.

n-hexane is more toxic than most hydrocarbons btw, nasty stuff, bee carefull not to breathe the fumes or have too much skin contact with it.

[UncleFester]

It's a hydrocarbon solvent pretty similar to heptane.

[WizardX]

O-acetate methods using  acetic anhydride or acetyl chloride.
tert-BUTYL ACETATE

http://www.orgsyn.org/orgsyn/prep.asp?prep=cv3p0141

Look at B, two moles of the acetyl chloride/pyridine complex + H2O ==> acetic anhydride
ACID ANHYDRIDES

http://www.orgsyn.org/orgsyn/prep.asp?prep=cv3p0028

This acetyl chloride/pyridine complex can also be used in O-acetate synthesis as in part C of

http://www.orgsyn.org/orgsyn/prep.asp?prep=cv9p0507

Finally, a 1:1 mole ratio of acetyl chloride with anhydrous ephedrine will react with the ephedrine's -OH predominantly. Excess acetyl chloride will then react with the ephedrine's -NHCH3

The oxygen atom on the -OH has a greater electronegativity than the N atom on the -NHCH3

[readyeddie]

Heptane are any crystallization solvent is not needed when using acetic anhydride if sodium borohydride is going to be used for the hydrogenation.To get rid of any excess acetic anhydride left after forming the ester just add a bit of water to it.The water turns the excess acetic anhydride into acetic acid.From what swim sees the ester is a clear looking oil.

[UncleFester]

The kind anyone just fooling around without evil intent, or even seeming a bit out of the ordinary, those are the best ones to use. That's why I did the acetic acid ester prep with sulfuric acid as catalyst. The Patent seems to make clear that this is a rotten way to make the ester in good yields. Ther was a posting in this forum using nitric acid as "promoter" for hydrogenation, and I think it came out of the Far East, where this synth is popular. I think I will hit THFSE and see what I pull up. Changing solvent to HCl in electrohydrogenation brings up that chlorine at the anode problem.

[readyeddie]

That's why I did the acetic acid ester prep with sulfuric acid as catalyst. The Patent seems to make clear that this is a rotten way to make the ester in good yields.

Sulfuric acid poisons palladium catalyts.

[Barium]

Sulfuric acid poisons palladium catalyts.

Under very specific conditions it can, but generally it sure doesn't.