Total 4-FA synthesis using Al/Hg reduction

IndoleAmine · Dreamreader Deluxe

Its a auto-censorship for words like this, due to bots searching our site for those words. You can still use n-methyl-phenyl-2-aminopropane for example.... Very Happy

Didin't you notice I mentioned the case of 3,4-methylenedioxy substituted phenylisopropylamines as being an EXCEPTION to the rule of diminished activity with lengthened N-alkyl chains, together with n-methylphenylisopropylamine itself?

Nice you mentioned it too, the more people talk about it, the more people will learn about it.

Sandmeyer · Fri Apr 22, 2005 4:38 am

IndoleAmine · Dreamreader Deluxe

IndoleAmine · Dreamreader Deluxe

And besides, its redundant anyway: because originally, I just wanted to remark that there are 2 exceptions where methylation enhances activity, and now I did so at least three times, thanks to your nonunderstanding.

As I said a few posts earlier:

tetraedr · Fri May 20, 2005 12:15 am

I want to present you some fresh data connected this theme.
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Stage 1. 4-FP2P.
9.93 g (44 mmol, 2.2 eq) of tin chloride was dissolved in 5.7 mL (1.5 g, 40 mmol, 2 eq) of HCl (in 250 mL Erlenmeyer flask), then was added 7 mL of water, 3.63 g (20 mmol, 1.0 eq) of 4-FPNP and 12 mL of toluene. Obtained clear yellow mixture was heated with reflux for 6 h with vigorous stirring. After cooling, a big amount of potassium carbonate was added carefully until the tough consistence of reaction mixture. Product was extracted 4 times with ethyl acetate, dried over sodium sulfate, evaporated under reduced pressure and finally thoroughly dried in vacuum. Yield – 3.05 g (100%) as yellow oil, which was used on the next stage without additional purification.

Stage 2: PFMA.
3.5 g of alu foil was amalgamated as described above. After washing with water, there was added solution of 1.96 g (35 mmol, 1.75 eq) of KOH in 15 mL of water, solution of 2.03 g (30 mmol, 1.5 eq) of methylamine hydrochloride in 15 mL of water and solution of 3.05 g of 4-PNP (20 mmol, 1.0 eq) in 30 mL of IPA. Slow exothermic reaction was occurred, the reaction mixture was warmed up, aluminium was dissolved, grey precipitate was obtained. Reaction was completed after 2 h, mixture was cooled down. The reaction mixture was filtered off, the filter cakes were washed with IPA and water. Filtrate was acidified with HCl until pH 1-2, concentrated for volume 1/3 from starting amount of solution under reduced pressure, diluted with water, washed 3 times with DCM, water layer was basified until pH 12-14. Product was extracted 3 times with ether, combined organic layers were dried with sodium sulfate, concentrated under reduced pressure, obtained clear almost colorless oil was diluted with IPA, acidified with HCl until ph=6, evaporated again, then co-evaporated 2 times with IPA, the residue was dried in high vacuum, then treated with dry ether, obtained crystals were filtered off and washed with ether and dried on air. Yield – 1.4 g (34%) – white crystals. M.p. about 90OC. Probably, it is better to do sulfate salt next time. The yield so low because the intermediate 4-fluorophenylacetone did not purified.
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I have got a new very positive and detailed biotest-data for 4-FA, its will be published here a little bit later.... Just waiting...

IndoleAmine · Dreamreader Deluxe

Awaiting bioassay & test results...

While reading about your crystallization technique, have you already considered using toluene(xylene)/dean-stark trap for dehydrating after adding aequ. HCl? Just dissolve amine in tolunene, add 1.01x molar amnt. of HCl, reflux until no more H2O separates in trap, then remove half of the toluene by distillation, then cool in fridge (sometimes it oils out), then decant toluene and add same volume of anhydrous acetone to cause the oil to solidify in a matter of a few hours (if it hasn't already)..

Otherwise: good work! Thumbs up!! Very Happy

(and yes - sulfate could be easier in this case)

Star-light · Blacklight bulb

mk-1 · Sat May 21, 2005 5:17 am

here are bioassays of 4FA from erowid

tetraedr · Sat May 21, 2005 8:43 am

SWIM has been tested 4-FA several days before, anf here I want to present this trip-report. Sorry for my bad english - my knowlegde of it can not permit me to express all these feelings after using this substance. But, I decieded, that publication of it as "raw-material" would be better, than nothing.

Saturday evening (real-time history)
19:15. 150 mg of subject was dissolved in 1.5 mL of water 150 and pushed in a muscle (with syringe).
19:20. The income is similar simultaneously to income of amphetamine and MDMA. There are elements of discomfort: anxiety, clenching the teeth, changing state from cold to fever. But these unpleasant feelings were lower, than after taking 150 mg of MDA. Also there were all elements (but more poorly) of methedrine income.
19:25 Elements of discomfort have disappeared, there is a smooth pleasant income (increase) of action.
19:30. Has left on a plateau.
This action really is similar on MDMA and amphethamine. Before, SWIM was tried only once time the mix of 150 mg of MDMA and 130 mg of methcatinone and, at that time, that mix has seemed not so good. Prevail methcatinone. Here it wanted for them and to be caught up. Probably, the problem was in a wrong parity(ratio) and selection of dosages of components. Also it was necessary to take amphethamine instead of methcatinone. And here all is rather well balanced. The dosagee has appeared normal, I think, that 200 mg it would be possible to sustain, but 200 – it is maximal (for specific SWIM)
19:50. The action, it seems, slowly turns into stimulator side. But, probably, it is subjective. Also, it seems, that the action hardly weakens. Probably, soon it will be necessary to be caught up. Only question than, when and how many mg.
19:55. The intensity of action (on peak), is similar to 120-150 mg of methedrine. Libido did not increased. The headache is not present, noise in the ears, practically, also left. It would not be desirable to lay, is active moving too. It is strange, but working on computer is possible – fingers are printing on keyboard almost normally. Usually, SWIM can not operate computer after MDMA or methedrine.
20:05. Action is really becomes weak. It would be desirable to be caught up really. Similar, that on duration of action is similar to methcatinone. But SWIM had angst for addition of new doze intravenously. In a mouth bad taste, similar to methedrine.
20:10. 100 mg of 4-FA was dissolved in 1.5 mL of water and was pushed in muslce.
20:20. The dispersal has passed more pleasantly and softly, than previous. It was, probably, because the dosage, or other reasons was less. There almost were not unpleasant moments. Would be It is possible safely to put 150 mg or more. Or intravenously. Sense to reduce a dosage special was not. But also it also has not broken off. Everything was normal. Again it wanted to lay in bed (MDMA-like action). (I have forgot to say that after MDMA SWIM normally lay in bed in relax). Voluminous allocation of sweat – was feel hot.
20:30. All is very good. Because of heat and sweats it was necessary to undress. Not clearly, that it would be desirable: neither to move, nor to not move. To sit and type on computer - normally. To lie down - it is also normal. To resemble - too it is good. But, is felt, that euphoria is small. One more 4-FA? But … It already next time. Next time already will be be precisely was clearly, as, where and on how many. It is possible for them, all night using only on 4-FA, periodically being caught up.
20.45. Continue to surfing in Internet. Though, it would be possible to do many different things. And even, it is possible to go to the party or to disco. Nothing can break this good feeling. But all the same, already it is time to be caught up. By something more serious (pure methedrine?). Now SWIM shall begins preparation for this…
21:00 End of a series of 4-FA.

The data about bioassay of PFMA will be later. It is waiting for volunteers.

tetraedr · Wed May 25, 2005 12:09 am

I want to anounced two good news.

First: The people, who tested PFMA were alive!
They wrote a very big trip-report and it is in translation to English. Now I just can say, that this experience was very positive, too. Short to say, the action of this substance something between amphethamine and methamphethamine, duration is about 10 h (close to amph), with light empathogenic effect.

Second:
Here is NMR-spectrum of PFMA:
NMR-1H (DMSO-d6) ppm: 1.09 d (3H, Me), 2.53 bs (NMe +DMSO), 2.64-2.70 m (1H, CHa), 3.19-3.24 m (1H, CHb), 3.45 bs (1H, CH), 7.11-7.16 m, (2H, Ar-CH), 7.27-7.31 m, (2H, Ar-CH), 9.36, bs (2H, NH2+).

grandpa · smurf

Star-light · Blacklight bulb

Stinging_Nettle · Sat Jun 11, 2005 3:49 pm

maybe try some 4-chloroamphetamine - that should be fun

joe_aldehyde · huxleys associate