I was looking at this, from http://www.lycaeum.org/leda/Documents/2C-B_Synthesis.11171.shtml

 The first procedure is to change the 2,5DMB into 2,5-dimethoxynitrostyrene. We do this by heating a mixture of 2,5DMB and nitromethane in the presence of a catalyst, ammonium acetate. Set up an apparatus for refluxing. 'Refluxing' is basically boiling a solvent in such a way that the solvent continually evaporates, condenses, and is returned back to the boiling vessel. To do this we set up the apparatus as shown.

Diagram of reaction vessel with reflux condenser goes here

Place 100 Grams of 2,5DMB into a 500ml flask and add 200grams of nitromethane. Most of the solids should dissolve but if they don't immediately, don't worry - they will once you start heating them. When most of them are dissolved, add 10 grams of ammonium acetate. Place the flask into an oil bath on an electric hotplate, connect the condenser and start a slow water flow through the condenser. DO NOT use open flame in any of these procedures. Nitromethane is very flammable! It is, in fact, rocket fuel. It's dangerous enough using an electric hot plate because of the sparks produced when the thermostat clicks on and off, but if you keep reasonable ventilation and a watchful eye on things, you should be okay. Turn the stove up to about 100 degrees celsius, the boiling point of nitromethane, and adjust it until the solution is boiling nicely. In a short time the color of the solution will turn yellow. Four hours later, when you are done refluxing, the color should be a deep red.

Immediately set up for vacuum evaporation. If you let the solution cool off too much it may spontaneously crystalize, making it more difficult to purify, so do a little planning ahead of time. Turn the heat off, detach the condenser from the flask and add a few boiling chips to mixture. Boiling chips provide a very large surface area for lots of small boiling bubbles to form. This will keep the solution boiling smoothly without any "bumps" or big erratic bubbles. Connect the vacuum hose and apply a vacuum very gently at first and build up to a rolling boil without boiling up into the hose. As the solution evaporates, the flask will cool down and you will have to adjust the heat of the hot plate to keep a steady boil going. Eventually, you will remove enough solvent and the whole mass will crystalize into bright pumpkin-orange crystals.

Turn off the heat and remove the vacuum hose from the flask. Always remove the hose from the flask before turning off the water. Otherwise, as the pressure drops water may be sucked into your product. Add 100ml of boiling isopropyl alchohol (IPA) to the mass and stir it as well as you can, breaking up all of the clumps. Your hot plate may still be hot and if you are working near it be sure NOT to splash any of this nitrostyrene onto the hot surface. The resulting fumes are a very potent teargas, something you don't want to experience! Let the flask cool and then pour off the red-colored alcohol solution. Add another 100ml of boiling IPA to the crystals and rinse as before. Rinse at least two more times or until needle-like crystals form out of the amorphous orange mush. Filter these crystals off and air dry completely. There must not be any alchohol left in the crystals, as this will ruin the lithium alumnium hydride (LAH) in the next step. This is 2,5-dimethoxynitrostyrene (2,5DMNS).

Could this be substituted with 3,4,5 TMB instead of 2,5 DMB in the same ratios?  If the ratios are to be different, how is the way to calculate such?
Also, is the vaccum necessary to remove the solvent?   I have an aspirator that i think could maybe do this, but I am concerned about the fumes from this being too smelly for kitchen chemistry.   Could this just be left out for a few nights in a shed or the like to evaporate?   Could the nitromethane being vaccumed off be reclaimed by distillation or is that too dangerous for a newb?


Thanks for your time

p.s. also found this while poking around

    * 250g 3,4,5-Trimethoxybenzaldehyde
    * 500ml Nitromethane
    * 10g Ammonium Acetate (anhydrous)

Procedure

    * Gently reflux for 5-6 hours
    * Cool and distill off any residual nitromethane.

          If the crystaline mass prevents distillation, remove it by vacuum filtration and use what is collected OR distill off the filtered nitromethane solution to collect an additional crop of crystals (If the crystals are stuck in the flask skip to the next step).

    * Add enough boiling MeOH to dissolve the entire mass (If it's stuck in the flask, if not skip this step, filter, and recrystalize once from boiling MeOH)
    * Decant, cool and vacuum filter, repeat the recrystalization if the crystals are not a pure yellow color (which they usually are).

Gently reflux at about what temperature?  just to where it's boiling a little?  Does the Nitromethane need to be distilled off?   Could i not just suction this off in a buchner funnel or something without dealing with vaccum or distillation of something like nitromethane, as it suggests later?

To prepare ammonium acetate in the anyhydrous form- one leaves an amount of ammonium acetate in a dessicating chamber with dry NaOH or the like, hm?   For how long?

Yeah, I'm clearly a newb.   Pardon my newbishness.

Yeah, my main concern at this point is blowing myself up during the reflux.   Being splattered all over some garage wall is not a good look this season.
I have a hotplate and stirrer, and proper equipment for everything, even a couple of thermometers to keep an eye on the heat and everything.   Nitromethane boils at about the same temperature as water, so I ran a reflux in an oil bath on some water today (it was thrilling!) and was able to manage keeping it at the correct temperature and the reflux under control.

I don't know for sure that this means that i'm ready to move on to the nitrostyrene from 3,4,5 thing or not just yet.

Once I allow the crystalline mass to cool, it's just a matter of using a buchner funnel to filter off the Nitromethane?   Can that be saved and used for later, or is it pretty junked up by the reaction?  Will the resulting orange crystals need any further purification before reducing?

Anything I should maybe look into before moving forward?   I'd hate be a tragic case.  What would be better than a mescaline synth to start with?   I have very little interest in bringing something like tweak into this world.

i do happen to have a bunch of vanillin just laying around... (it really smells wonderful!)
got any gentle nudges in the right direction in regards to that one?

but why use the nitromethane as solvent in the first place? it is a waste of material. you can use instead a procedure which is conducted in methanol or ethanol or isopropanol, with some amine catalyst, prefrably neutralized with acetic acid. the 2,5-dimethoxybezaldehyde really likes ethylenediamine diacetate, procedure can be found in rhodium's archive.
Cant remember off hand if 3,4,5-TMB also likes this particular amine, but trying out small quantities with several amine+acetic acid is a good idea. methylamine is an especially good amine catalyst, when used in 5-15% (relative to the aldehyde) and neutralized with acetic acid for a variety of nitrostyrenes/propenes. butylamine iirc also was used with success.
just dissolve the aldehyde in choice of alcohol (might require slight heating in case of solid aldehyde), add 5-15% amine acetate (or equimolar amounts of amine and acetic acid), add nitroalkane, boil to reflux (reflux temp would be that of the alcohol) for 45-90 minutes, let cool and stuff in the freezer for crystalization.
you know youre using the right amine for your aldehyde when you see that reaction takes no more then 1.5 hours. a good visual aid to know when to stop the reaction is, as soon as it darkens. it may change color, say from yellow to orange, colorless to yellow, etc... , but as soon as darkness/redness sets in its allready a bit too late.
other way ofcourse is to use TLC to see when all/most aldehyde reacted.

sorry for long post.

Trimethyl phosphate is very efficient at alkylation of syringaldehyde and vanillin, I have experience with both reactions. Also i have made 3,4,5-trimethoxyphenethylamine from vanillin, it's very easy, assuming you have experience and chemicals/glassware needed. As for the person starting this thread just reading what you are posting itis clear you should probably try something else first, or practice some general chemistry involving the sort of reactions you will be doing. Better yet, make some simple phenethylamine from a different benzaldehyde.
All this talk about the nitromethane, well first off using half a liter or whatever as solvent is just stupid, because it's an unnecessary risk and waste of reagent. No, I am not saying Sasha is stupid. All you need is IPA, 1.1eq nitromethane to benzaldehyde, your catalyst which the best for this benzaldehyde is cyclohexylamine. You can use others too, EDDA, butylamine as said above. The point is, you absolutely do not need so much damn nitromethane!
I would suggest something like this, get some vanillin and methylate, or buy 3,4-dimethoxybenzaldehyde. From here practice making a nitrostyrene, you can then practice reduction. Upside of this is practice first and foremost, and legality. You can buy vanillin and alkylate with easily made alkyl halides such as isopropyl bromide and ethyl bromide. Make the corresponding nitrostyrene etc. After you have made a few and educated yourself further you might find mescaline is easy. But of course, this is all just my opinion.
I should also mention you can make the nitrostyrene by the cold method, I've used it on 3,4,5-TMBA, it works well. It is safer, more straight forward and used little nitromethane. It also gives a nice bright yellow product even prior to recrystallization. As for reduction, Zn/HCl does work but yields are always erratic from trial to trial.

 ^^^^I dunno bout that method with 3,4,5 TMB? I've done this with other subbed benzaldehydes with some great yields (but it gets fucking messy and too much liquids at larger scales!) but had heard that 3,4,5 TMB didn't respond as well to making and dehydrating the alcohol, etc. I tried 3,4,5 TMB with Ammonium acetate (ok) and cyclohexylamine (much better). Never tried it with EDDA either, and couldn't find any hard data from anyone that had. 3,4,5 TMB is a bit pickier than  other subs.. ,.still very manageable. If dude then had a Parr, he'd be in business. .

Hell that is more than good enough. I wouldn't get much better than that using AA, so that it makes it viable. Considering how cheap and easy 3,4,5 TMB is to get, that presents no problem. It gets manufactured in insane quantites in China for use in some antibiotic synthesis, so it can be had by the Kg for nada..

what's an EQ?  equivalent quantity?

USE THE FUCKING WIKIPEDIA !!!

h**ps://secure.wikimedia.org/wikipedia/en/wiki/Equivalent_weight

 

I was walking along, and I found an old Journal in the Library stacks, and it read as such:

"The procedure from Vanillin to 3,4,5-Trimethoxybenzaldehyde is a simple one to do upto the Alkylation point of 5-OH-Vanillin.

The attempts at non-stirred, insufficiently basified (NaOH) catalyzed condensation of Vanillin with Nitromethane, in a room temperature environment was successful, yielding a beautiful yellow nitrostyrene product, though it was at best 30% yield.

Those that have a fear of explosion/detonation/refluxing of Nitromethane should sincerely give the references for a cold/room temperature condensation a glance."

As a comment about the variable yields run to run on the Zn/HCl reduction of the nitrostyrene by pyramid, was the zinc activated/cleansed from it's oxide covering?

Thanks for elaborating pyramid. I think that NaBH4 would be preferential for most reductions, but the hassle of obtianing for most is a deterrent.

As for the condensation, no, it was not a typo, the condensation was performed on vanillin since it was not available for that to be attempted on 3,4,5-Trimethoxybenzaldehyde, as there was none. It was just a report of some goofing off apparently, in an attempt to add more, if not slightly skewed subject experience.