no dealing with gasses you have to consider
1) leaks
2)moisture generation
3)suckback
4) rate of absorption/dissolution
5)foaming
stuff like that, it really does'nt matter how you rig up a gas generator, you just have to keep all  those variables in mind.
you can use fancy glass but if it is'nt sealed properly no dice.

There is a thread i checked out on sciencemadness (its from 4 days ago) where they talk about turning primary and secondary halides into their corresponding aldehydes and ketones using nitromethane instead of nitropropane!

Don't waste your time on this synthesis approach. Go via Alkene, -C=C-CH3 to Ketone, -CH2-C(=O)-CH3

Preparation of nickel-oxide hydroxide electrode http://www.freepatentsonline.com/4462875.html | http://www.freepatentsonline.com/4462875.pdf

Why turn the halide into the ketone? The halide usually gives better yields, last I checked.

For ketone + amine ==[imine]==[catalytic hydrogenation]==> amine (95%+) http://www.erowid.org/archive/rhodium/chemistry/reductive.alkylation.html

Imines are sometimes difficult to isolate and purify due to their sensitivity to hydrolysis. http://www2.chemistry.msu.edu/faculty/reusch/VirtTxtJml/aldket1.htm

Synthesis of the imine is the limiting reaction, therefore, the method below.

---

A Simple One-Pot Synthesis of Functionalized Ketimines from Ketones and Amine Hydrochloride Salts.

Abstract
Functionalized ketimines of the general formula RR'C(=NCH2Y) [R and R' = Ph, alkyl; Y = CN (1), CH2Cl (2), COOMe (3)] have been prepared by the condensation of ketones with the corresponding primary amine hydrochloride salts [NH2CH2Cl.HCl (4), NH2CH2CH2Cl.HCL (5) and NH2CH2COOMe HCl (6), respectively]. The reported reaction proceeds mildly in a single step without the need of a previous isolation of the free amine from its salt. N,N-Dimethylformamide (DMF) is used as the solvent and TiCl4 as the drying agent.

http://www.informaworld.com/smpp/952799086-72057594/content~db=all~content=a756986657

BUt which method do you suggest for catalytic hydrogenation? I've wondered, without giving it too much thought i have to admit, how one could do this kind of reaction with OTC stuff.

The Leuckart is basically transfer hydrogenation, just without any catalyst -- methylammonium formate is worth a look.

the problem with leukarts is they are touchy and yeilds are only 60% or so.
it's too much hassle to watch a thermometer for 30 hours and adjust the rheostat accordingly when you can simply mix a and b together to get c.

Indeed. If I had some P2Pol, I'd probably just HBr it to the bromo-compound (PiPBr?) and go from there.

I'll hopefully be diving into some electrochemistry here shortly.

There seems to be a bit of a shortage of actual writeups and reports from others. It's one thing to read about something as touchy as EC in a peer reviewed journal as it happened in a university lab - it's another thing to hear about success in somebody's garage.


A bit OT, but safrole -> MDX(X) is already possible OTC, assuming one has the safrole. GAA is OTC, it's the safrole which just can't be had in North America, Western Europe, and Australia. MeAm from OTC hexamine hydrolysis, formaldehyde/NH4Cl, or a NM reduction.

No I wasn't referring to jon's method....not quite sure which one that is.

As for electrochem, I'm sure it will become substantially less complicated to me as soon as I can hold it in my hand...personal thing.

Pure GAA has several OTC sources. The most common is at photography supply stores, where it is sold as a dilutable stop bath ingredient. This isn't suspicious, because most professionals don't like paying for a giant bottle of mostly water.

There are a few others, but they aren't as common, and I'd hesitate to mention them in an open forum.

Both formaldehyde and NH4Cl can both be found at a Wal-Mart, a well-stocked hardware store, or a well-stocked agriculture supply store. You'll find formaldehyde as formalin solution in pet stores. You'll find it as paraformaldehyde at outdoors stores. NH4Cl is all over the place, from welding supplies to homebrewing stores.

down under they sell paraformaldehyde as a septic disenfectant for camper toilets it contains surfacants that can be washed away with water on a buschner funnel.
then it's ready to use after drying, ammonium chloride is easy to find.
the two things to keep in mind temperature must stay right at 106 between 104-106
and pull just a slight vacum until you see all the co2 bubbling from the top.
this way all of the ammonium chloride converts to methylamine and it makes workup a breeze because of purity and yeild.