Author Topic: MDA with NH4OH  (Read 1653 times)

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methlab

  • Guest
MDA with NH4OH
« on: April 03, 2004, 09:23:00 PM »
Hi! I'm a little bit confused, i used TFSE for an MDA recipe, found some using NH4Cl and some using NH4OH (ammoniumhydroxid, in my case 25%). The problem is that some bees say that it is not possible to use NH4OH some say it is. Can one clearify this please. Otherwise it should be possible to make some NH4Cl by reacting NH4OH with HCl, right? Greetings

Rhodium

  • Guest
Find another route
« Reply #1 on: April 04, 2004, 02:50:00 AM »
If you UTFSE some more, you will see everybody telling you that any MDA "recipe" using ammonia or ammonium chloride is useless (yields ~25%)...


amine

  • Guest
why not use hydroxylamine?
« Reply #2 on: April 06, 2004, 06:18:00 AM »
why not use hydroxylamine?
make the oxime and then reduce it via al/hg.
look on rhodium's main page for it.

Organikum

  • Guest
ammonia for reductive amination
« Reply #3 on: April 06, 2004, 03:43:00 PM »

you will see everybody telling you that any MDA "recipe" using ammonia or ammonium chloride is useless (yields ~25%)...



Huh?
The (book) ORGANIKUM, 21ed, page 585, states 90% yield for the reductive amination of P2P to amphetamine using ammonia in methanol and Raney Nickel under pressure.

The use of a platinium catalyst should avoid the high pressure (3atm instead of 100atm) and give similar yields.

But I maybe wrong of course.




Rhodium

  • Guest
Possible, but still not easy
« Reply #4 on: April 06, 2004, 04:09:00 PM »
Yes, that is probably correct, but high-pressure catalytic hydrogenation isn't part of the misleading writeups out there which makes newbees hope for an easy MDA synthesis using ammonia.

I do not dispute that it was possible to achieve a high yield, I only meant to say that such a procedure for MDA isn't in circulation.


starlight

  • Guest
These posts may be of interest to you
« Reply #5 on: April 06, 2004, 06:34:00 PM »
One is done anydrous, the other wet.

Post 485344 (missing)

(Lego: "Reductive amination with Ti(iPrO)4/NaBH4", Novel Discourse)

Post 335851

(Sunlight: "MDA and MDMA from CTH reductive amination", Novel Discourse)

methlab

  • Guest
MDA via TCBOE Chapter 7 ???
« Reply #6 on: April 06, 2004, 06:41:00 PM »
Hi! Rhodium you told me that every ammonia reaction has a very low yield. Is the following writeup on your page wrong? (

https://www.thevespiary.org/rhodium/Rhodium/chemistry/tcboe/chapter7.html

)

Aluminum Amalgam Reduction[from chapter7, TCBOE]

72.5g of aluminum foil is cut into one inch squares and placed into a 3000ml erlenmeyer flask or other suitable glass container. A solution of 1.8 grams of mercuric chloride (HgCl2) in 2530 ml water is added, and the mixture is stirred occasionally over 30 minutes to amalgamate the aluminum. The solution is poured off and the foil is washed with four one-liter portions of water.

To the amalgam is added, in sequence, 80g of ammonium chloride in 101ml of water, 302ml of isopropyl alcohol (100%), 244ml of 25% NaOH solution, 89g (0.5 moles) of piperonylacetone, and then 588ml of isopropyl alcohol. The mixture is swirled occasionally for two hours, and kept below 60°C by cooling with an ice bath as necessary.

The mixture is then filtered through Celite (a diatomaceous silicate powder which is placed in a layer over the filter paper before filtering, it is sold by chemical companies as Celite), and the filter cake is washed thoroughly with methanol. Combine the liquid filtrates and distill off the methanol (65°C), isopropyl alcohol (82°C) and the water (100°C).

Dissolve the oil in 200ml of ether, and extract the MDA into two 500 ml portions of 3N HCl. The acid solution is washed with three portions of methylene chloride equal in volume to the acid solution (you will probably have to wash portions of the solution at a time unless you have a huge separatory funnel). The acid solution is basified with excess 25% sodium hydroxide solution (red litmus turns blue) and the liberated oil is extracted into three 500ml portions of methylene chloride.

The methylene chloride solution is dried with magnesium sulfate. The drying agent is filtered out and the methylene chloride distilled out. The residual oil is distilled under reduced pressure and the distilled oil then dissolved in ether
(or toluene or methylene chloride). HCl gas is bubbled through the solution until no more precipitate is formed. The precipitate is filtered off and allowed to dry (~70% yield can be expected).

Has one tried this? If it's wrong, this seems to be a misinformation.

greetings

starlight

  • Guest
you would find it a lot quicker to search
« Reply #7 on: April 06, 2004, 07:09:00 PM »
you would have to spend less time if you used the search engine at this site.

just typing "tcboe" (no quotes) into the search engine gives you the info you need. have a look at the following post

Post 443143

(Rhodium: "TCBOE is in error - again.", Serious Chemistry)

Organikum

  • Guest
Not everything on Rhodiums page is - up to...
« Reply #8 on: April 06, 2004, 07:13:00 PM »
Not everything on Rhodiums page is
- up to date
- right

The page is a collection of older and newer information and some things SOUND right but at a nearer look they are untried/bogus. For verification of the information you may consult the scientific literature and the HIVE. Here people report their experiences, thats the reason why this board exists.

There is no silverspoon, but there is a search engine.
UTFSE !

To the synthesis from TCBOE (a quite antique book btw.):
It seems to me that the author took the procedure for reductive amination of another compound - an hydroxyphenylacetone for example - and used it for this "writeup" without trying it and without realizing that there are big differences from compound to compound. To stick to the example, hydroxyphenylacetones form stable imines - phenylacetones dont do so. And so would this procedure probably work on phenylacetylcarbinol, but it wont work well on (MD)P2P. This was tried here at the HIVE and can be regarded as proven.