At normal temperature the dissolution is much slower – several days are needed. A’s trial and error regarding this reaction’s parameters. Another mL of toluene was dumped in the beaker and thoroughly mixed. Alternatively, you could filter it through a paper towel, but you will still lose the same amount when the towel absorbs it. My yields were awesome and the purity was excellent. The gallum is One thing that I want to mention in hindsight here since I know it’s probably going to come up, is the issue of added water.

The Wolf agreed, but insisted that they modify the procedure ever so slightly. Masaru Yamada, Kansai University, and Dr. It will probably take about 4 to 5 “loads” in your grinder to do the whole 25g of foil, depending on the size of your grinder. Closeup of foil balls Figure 4: I put 5g batches into a small Braun coffee grinder and ground the foil for seconds. And lo and behold there was another massive precipitation of crystals. Triethylamine has been used during the synthesis of:

Then after a few minutes you will see them joined by larger bubbles closer phot the size of those seen in boiling water. Sludge In BeakerFigure I would expect there to be some remainingMDPP with its slight color, or for some reaction impurities to give a color too.

a photo essay on the nitromethane al/hg

Swirl it a couple times and give it about 10 minutes to cool down to something closer to ambient temperature. Weep with joy as a bumper crop of white precipitate crashes out of solution.


Everything else tookcare of itself.

Reductive Amination of MDP2P with Al/Hg + Nitromethane

There was probably no more than about 15 mL of toluene left floating on the sludge in the beaker when I was done. Into a separatory funnel no smaller than mL capacity, pour your nice gray reaction mixture, being very careful to keep the stirbar from falling into the sep funnel and breaking it that would be ugly. I did the whole reaction, with crystallization, in the span of an evening. Basifying should be a gentle process. Synthesis of five- and six-membered nitrogen-containing heterocyclic nitromethane,12’52 bromonitromethane,23 47 and methylamine, butylamine.

They added it over a 5 minute period of time.

A photo essay on the nitromethane al/hg

Volume developed using both N-benzyl-N-methylamine and 2,3 of aldehydes and nitromethane was established using. They are as follows:. I set up a two-liter flat-bottom three-neck flask, and plugged one of the necks. The final, overall iBT score ranges between 0 andand includes a scaled average from the four components reading, listening, speaking, and writing. A’s trial and error regarding this reaction’s parameters.

Photo Essay of Reductive Amination by – Instruction manuals

Therefore this writeup will illustrate the reaction on a scale of It will reach this state at about one hour 45 minutes to two hours after addition was started. If you have prepared the foil as described above, it will easily stir. Snoopy freaked out, ran and got an ice bucket with ice nitromethae placed the beaker on ice for a few minutes until the reaction was under control a matter of minutes then the beaker was placed back on the stirrer and the reaction allowed to continue for 3 hours.


But this was slightly milky white.

Reductive Amination of MDP2P with Al/Hg + Nitromethane

It had been distilled srcinally, still smelledgood and was a medium-light green color. We are nonprofit website to share and download documents. Everything else took care of itself. It warmed up slightly but not appreciably. This mixed the two phases well. About 4 pounds of ice in 2. Shake it a few times during this period. Acid is also not absolutely necessary in reductive aminations of aldehydes or ketones.

Set this solution aside. Methylamine With Etoh – Download as. Just be vigilant while pouring the last 50 mL or so and avoid letting that glob of crap rejoin the toluene. I then left for about an hour to let the reaction finish itself. Some pieces hadstarted to float.

a photo essay on the nitromethane al/hg

Incriminating, to say the least, but I am his attorney, ao/hg all, and attorney-client privilege is a powerful thing. When the mixture in the sep funnel has cooled down, extract it once with mL toluene followed by once with mL toluene.