A was adding about 25 mL, and maybe it was not a good thing. This worked amazingly well. Gas began to come out of the dispersion tube, which I immersed in the toluene filtrate. After several unsuccessful attempts I have come to the conclusion, that if I preheat the gallium in oven in a crucible at around C the Al-foil is easily dissolved in the gallium. Acid is also not absolutely necessary in reductive aminations of aldehydes or ketones. The garbage bottom layer was removed and the top layer was transferred to a flask and the methanol evaporated leaving the impure amine. I suspect this will work fine.

Then add 55 gm of aluminum squares appx 1″ sq that have been cut from pie tins. Methylamine is an organic compound with a formula of CH3NH2. This document deals with the preparation of Methylamine and Methylamine constant nagging of others, I am including a route based on the reduction of Nitromethane. I made a little mistake: Since the appearance of Ritter’s writeup of this method in Total Synthesis II, much discussion has taken place about it but, it has sometimes seemed. You will probably even need to add an extra mL of MeOH down the condenser at this point or before to help it keep stirring effectively.

They are as follows: In less than 10 minutes, faint bubbling was visible, the solution was gray, and the aluminum was distinctly less shiny. It was then filtered into a new beaker also super dryand the MgSO4 in the filter washed with a little new toluene. Another point I would like to make about the timing of the addition against the breakdown of the aluminum is that Mr.


Melgar Anti-Spam Agent Posts: The dropping funnel was put on a side neck on the flask.

a photo essay on the nitromethane al/hg

Sorry, I missed that in the first read. Turn the stirring on full blast for a 5-second burst to intimately mix the solution and the foil.

Volume developed using both N-benzyl-N-methylamine and 2,3 of aldehydes and nitromethane was established using. This document deals with the preparation of Methylamine and Methylamine constant nagging of others, I am including a route based on the reduction of Nitromethane. I observed firsthand the trials and tribulations of Mr.

Sun, 21 Jan By using our site, you agree to our use of cookies. In other words, you have to watch niyromethane two nitrimethane and sort of adjust the addition so that they proceed at approximately the same rate.

Photo Essay of Reductive Amination by Dr.gonzo

GonzoJust the other day, I received a most interesting package in the mail from one of my clients, who we shall callRaoul Duke.

When you can feel exothermic warmth begin by feeling the outside of the flask, quickly add about 2. That is to say, maybe there is some trace water in the MeOH Mr.

I mixed mL of water and g of NaOH in a beaker. A uses Heet that is fulfilling this function, and maybe it’s even in all MeOH except expensive absolute anhydrous stuff. Gazeta Do Rzeczy Nr. One reason I bring this all up is that there has been lots of talk about how this reaction needs 8 hours or 24 hours or even 36 hours to run!

A photo essay on the nitromethane al/hg

At normal temperature the dissolution is much slower – several days are needed. At first they will be tiny, like champagne bubbles. Therefore this writeup will illustrate the reaction on a scale of The mix was starting to get very viscous, so I added another mL of MeOH down thecondenser which greatly improved things.


The reduction ran hot but was completely easay control, easily stirred, fast, and simple to work up. When I got back things had cooled considerably and the mix was mostly an amorphous gray with just thetiniest flecks of white mixed in. Shake it a few times during this period.

A Photo Essay on the Nitromethane Al/Hg

Originally posted by laserlisa. Masaru Yamada, Kansai Phoot, and Dr. About every minute, I turned on the stirrer for about 5 seconds. I would expect there to be some remainingMDPP with its slight color, or for some reaction impurities to give a color too. You will also see sludge already starting to settle at the bottom and forming a ring on the glass around the top surface of the spinning mess.

I suspect this will work fine.

a photo essay on the nitromethane al/hg

nitromethahe It had been distilled originally, still smelled good and was a medium-light green color. The valve on the dropping funnel was opened so that the mix started dripping ataround one drop per second.