malvaxman (Hive Bee)
10-03-02 07:15
No 363703
      Ephedra extraction failure  Bookmark   

Some ephedra extact 8% was put in a glas on top of it was pured denat. EtOH. At this moment there was plenty of ephera sludge in the bottom of the glass but the upper part of it was pretty clear. The guy performing the experiment thinked: If I adjust the pH to about 12 there will form a layer of ephedrine at the top. This could then be colected with nonpolar, then the nonpolar could be sucked of and filtrated ect.
When adding the base there formed some white fluffy substance at the top of the vessel.tongue
Then the nonpolar shoud be added..., the guy had toluene.
Unfortunatly the toluene didnīt like to follow the rules of nature as the guy have expected it to do. The toluene sank to the bottom of the vessel where the rest of the ephedra crap was taking the good things with it. crazy it didnīt form any separable layers, toluene almost mixed entirely with the ethanol! shocked
Does the laws of nature only work like this where the guy lives? What should the guy do next according
to you?

The toluene was 99% labgrade.

(Chief Bee)
10-03-02 07:41
No 363706
      Toluene and ethanol are miscible.  Bookmark   

Toluene and ethanol are miscible. For two layers to form, you need to have two immiscible liquids:

(Hive Bee)
10-03-02 13:40
No 363858
      seperation woes  Bookmark   

You could mix it with lots of water and the toulene would seperate and float to the top, but the water would also turn the ephedra into goey slimey stuff. Everythings always a trade off!

Real Men Don't Preview Their Edits
10-03-02 21:17
No 364061
      Will a mere solvent extract react?  Bookmark   

Not yet tested from fear of wasted react.

But read this from ../rhodium/chemistry /ephedra.html

Approximately 425 grams of ground ephedra plant material was washed three times with methanol. The methanol washings were collected and allowed to evaporate to produce a greenish-brown tar-like substance. To this material was added 250 mL of a 57% solution of hydriodic acid and 9.5 grams of red phosphorus in a 1000 mL round-bottom flask.
...The reduction of ephedra with hydriodic acid and red phosphorus results in the production of d-methamphetamine, d-amphetamine, and d-N,N-dimethylamphetamine[8,13-15].

Is a 3xmethanol wash is all thats needed? Granted you wind up with a few extras in there but the presence of d-amph isn't of great concern and the article details that DMA traces are tiny.

(Hive Bee)
10-04-02 10:33
No 364245
      Isolation of l-ephedrine from ephedra
(Rated as: excellent)

100 g of coarsely powdered ephedra are added to a solution of 50 g sodium carbonate in 150 ml water. Liquid and powder are thoroughly mixed by means of a glass rod in a 1000 ml beaker and left there sitting for 2 hours.
Then follows the percolation in a percolator, but a Hempel column with a cork and a stopcock is a perfect substitute for this !
Percolator in the lower end  (just in front of the stopcock) is closed with a pad of glass wool, on which rests a bed of sea sand about 10 mm thick. Percolation tube is then filled to about 1/3 of its length with dichloromethane. The crumbly paste obtained from ephedra and sodium carbonate solution is then transferred into the percolator (stirring with glass rod is necessary to drive out air bubbles). The drug is tamped with glass wool and continously percolated with 1000 ml dichloromethane.
The percolate is rotovapped to a volume of about 5 ml. To the so concentrated extract 30 ml of ether are added and the ethereal solution is extracted in a sep funnel with 3x 50 ml 0.5 N hydrochloric acid. The acidic extracts are pooled and are filtrated over 50 g potassium carbonate in a funnel equipped with a fluted filter paper. The now neutral to slightly alkaline solution is then extracted with 4x 75 ml dichloromethane. The extracts are pooled and dried over anhydrous sodium sulfate.
The dichloromethane is distilled off and the residue, a yellow-orange oil, is dissolved in a mixture of 20 ml of ether and 20 ml of dichloromethane. The solution is then gassed with HCl, made from 20 ml of concentrated sulfuric acid and 10 g sodium chloride. The gas is dried by passing through a wash bottle filled with 50 ml of concentrated sulfuric acid. Excess of HCl is absorbed in 10 % NaOH-solution.
After about 10 minutes of gassing a dirty-white precipitate forms, which consists of ephedrine hydrochloride + the hydrochlorides of the other ephedra alcaloids. The gassing is then stopped, all tubing connections are taken apart and the raw alcaloid hydrochlorides are filtered (buechner funnel). The raw alcaloid salts are mixed with 30 ml acetone in a 250 ml beaker and heated to boil on a water bath. About 10 ml of methanol are then added, the salts must have gone totally into solution. A spatula tip full of activated carbon is added (carefully, the solution might spontaneously foam up and boil over), the solution is brought shortly to full boil and is then filtrated hot.
From the hot filtrate (in my experience it is best to bring the filtrate again to a boil and then take it from the water bath) the ephedrine hydrochloride is precipitated by adding acetone until crystals begin to form and letting the mixture cool to room temperature. After 6 hours of standing the precipitated ephedrine hydrochloride is filtered off, washed with a small volume of acetone and dried.
If the product shows impurities (testing is done by TLC), it is recrystallized by dissolving in 15 times its volume of methanol, adding about 100 times its volume of acetone and letting the mixture sit in the refrigerator for 6 hours at 4 °C. The then precipitated crytals are filter off by means of a sinter glass filter. After one or two recrystallizations no more impurities are shown by TLC.
Yield: varies from 0.5 g to 1.5 of ephedrine hydrochloride
TLC: silca gel 60 F(254 nm),  eluent consists of 49 parts ethanol, 49 parts dichloromethane, 2 parts ammonia solution 25 % (all parts by volume)

[Translated from:
Stahl/Schild: "Isolierung und Charakterisierung von Naturstoffen"; 1986, Fischer Verlag.
Italics mine]
[edit: The ephedra species used was ephedra sinica STAPF]

Quidquid agis, prudenter agas et respice finem!
(Hive Addict)
10-04-02 17:51
No 364351
      start over  Bookmark   

Evaporate to dryness and start over.

Here's an old, simple way, that will get you a concentrate with which you can easily deal.

Hell, it's way back in the search engine, but here's an update.

Just cover it in water and add HCl to pH 4 or so.

Heat just to boiling and cool (ice cubes).  Re adjust to pH 4.

If you are rich, evap to dryness and extract with alcohol,
if you are not, you can do it with water.

Richness and poorness are values dependant on personal circumstances, and the amount of ephedra you have.

Ah hell just use water.

Now you dilute the volume by some arbitray factor of 4, or 5, and you use a "sand trap" or "sand filter" (UTFSE) to filter the fluid.

If you have a suction set up this will go fast, otherwise, it won't.  ":<)

Re rinse the powder with water and repeat a couple of times.
as you will note, the brown water you collect  is now free of particulates.

any other way of attempting to filter this stuff will
be quite frustrating, and it was this particular extraction
that motivated the development of the sand trap (clandestinely) for Hivers and affilliates..

As you may note if in fact you DO UTFSE, there are some techniques, and filter media, that will enhance your results, which I refuse to repeat.

Were I to attempt this now, I would definitely condense the aqueous liquid to the gummy mess it becomes (using a microwave I would get it as dry as possible without burning it,) and I would proceed without fail to the techniques employed by VideoEditor and Geezemeister in their "dry extraction threads" where basing of the salt is done through acetone or naphtha SANS water, and precipitate the FB through the action of cold on the solvency of the base in the NP.  However, I would do this in a PP,  since I'm more or less attached (more, actually)coolto it's employment in hot flammable liquid operations.
(call me a dolt...??)crazy


However, since that way has some degree of speculativeness
associated with it (5 will get you 10 it would/will work like a charm, though..)

let us proceed archaically...winkso to speak..

(3 years IS a long time: ask Mr Clean..  )

Take your brown liquid and add NaOH or better, Na2CO3, to it, and some salt...

Now you can put your NP on top of that and shake the crap out of it and wait for it to settle.  But the emulsion will amaze you.  You can do whatever you want, but you will be stuck.

The best "old fashioned" way to do this step is to put the water solution in a ""glass"" or something inside an over flow tub, and fill it the rest of the way with xylene, and over flow it into the tub.

Now you can squirt the NP under the water in various ways, and as it rises it carries the FB with it and overflows into the tub again, and makes zero nada no emulsion.

someplace in UTFSE there is a big discussion about drop size volume vs area considerations, mass transport, and etc:

Mr Clean backed me up on it and ruined a couple of garden sprayers doing it, but then, he was way out of my nano natterings with his 5 gallon buckets and 50 lb loads..

If I were trying "proof of concept" tests, I'd probably just use your basic turkey baster, and hold the tip next to the bottom, so the NP would squirt out in a bunch of smaller drops, but if you were serious, you could get a peristaltic pump that could circulate the NP all night while you slept..

Anyway, friend, either way (and another one I'm not talking about yet...) it can be done quite handily, despite it's reputation for difficulty..

This is an essential repeat of some old posts, with an option for incorporation of new technology.  Sorry for the partial repetition...frown

09-18-03 14:59
No 459808
      A / B extraction  Bookmark   

I have a 5 pounds ephedra herbal is it possible to use this process "" for extract the ephedrine alkaloid ?