Greetings fellow nerds.
So this june has so far had very little actual progress despite a lot of work being done.
So first a brief recap.
I've been trying to make sodium metal by the alcohol catalyzed magnesium reduction approach and thus far i've been rather successful.
Turns out that all you need to do is mix together magnesium metal, sodium hydroxide, a percent of tertiary alcohol and use baby oil as the solvent.
Then you heat the mixture on a hotplate up past 200 celsius, preferably 340 celsius and stir.
After three days you get sodium metal.
Of course there is a lot of processing with dioxane to separate it from the slag but for the most part this process does work.
Unfortunately, there are some major issues.
One is time, spending three days per reaction to generate about ten grams or so of sodium is, to put it lightly, not a very efficient use of time.
That's one of the big reasons this month has been devoid of videos.
I've been wasting a lot of time on sodium related experiments.
I really need to build a second fume hood so i can do more experiments at once.
The second issue is damage and cost.
The reaction mixture is very damaging to glassware.
Expensive borosilicate laboratory glassware.
Sodium hydroxide is well known for dissolving silicon dioxide, including the silicon dioxide that glass is made out of.
In fact we exploit this property to make sodium silicate as shown in previous videos.
So i've been trying to figure out how to mitigate this problem.
The obvious and most straightforward solution is simply not to use glass at all.
Most ferrous metals, like steel, are completely immune to molten sodium hydroxide.
As well as a lot of non-ferrous metals like titanium and copper.
In fact among all the common metals, aluminum is probably the only one that's incompatible.
The other incompatible metals like magnesium aren't encountered that often as container materials.
But for now i'll keep using glass.
Glass lets you see what's going on and easily let's you stir the mixture by magnetic stirring.
So i'm going to need to figure out a way to protect the glass.
My first idea was to coat the glass with something.
Maybe a sacrificial coating of more glass.
After seeing the sodium silicate harden into a glass like solid in one of my previous videos,
I thought it might be applicable to my current problems with making sodium.
I poured in a small amount of sodium silicate, rolled it around until i got a nice coating, and heated it dry.
The small amount wasn't enough to crack the glass and it did indeed harden to a very hard and durable layer.
Unfortunately the boiling produces lots of obvious holes.
I think though this is still a promising route, perhaps the right mixture of chemicals can produce a thin solid cement.
But for now i'm going to put this route on the backburner and explore alternatives.
Now i know at relatively low temperatures the destruction of glass is fairly slow.
While highly susceptible substances like silica based cat litter can dissolve just at room temperature.
Quality borosilicate laboratory glassware is fairly resistant.
Unfortunately, running the sodium production reaction in mineral oil at modest temperatures around a hundred celsius doesn't seem to work.
Maybe the sodium alkoxide isn't reactive enough or maybe the magnesium isn't reactive either.
Whatever it is low temperatures doesn't seem to work.
At least the glass isn't destroyed.
But let's go with the hypothesis that the sodium alkoxide isn't soluble in mineral oil at these temperatures.
How do we solve that? Well, if we can't raise the temperature, maybe we can use a more polar solvent, something that can dissolve sodium alkoxide.
But we have to remember that sodium will be present and most polar solvents react with sodium, we need a polar solvent that doesn't react with sodium.
My first instinct was to attempt dioxane.
Dioxane is much more polar than mineral oil and also seems to have special properties for separating sodium from magnesium oxide slag.
Now this experiment already failed last year but at that time i didn't have the same insight as i do now
So i attempted the reaction again with stirring as well as a sodium metal jumpstart.
As usual i had sodium hydroxide and a stoichiometric excess of magnesium metal as well as a milliliter of tertiary alcohol.
In my case i used 3-ethyl-3-pentanol since i had such good results with it.
I let i run for a few days but nothing happened.
I also had a bubbler connected but noticed no hydrogen.
My reaction failed as before.
Oh well, it was worth a shot.
Now dioxane boils at about 100 celsius so maybe the temperature is just too low as per our theory.
We can't heat it higher or the dioxane would boil off.
So my next thought was to try and get a polar solvent that was higher boiling than dioxane.
Now we made dioxane using ethylene glycol, how about we use propylene glycol and make dimethyl dioxane?
I couldn't find reliable literature data on the boiling point but i thought it would be higher and worth an attempt.
Unfortunately i thought wrong.
I got myself some propylene glycol based antifreeze and proceeded to condense it to make dimethyl dioxane in a very similar fashion to making regular dioxane.
I mixed it with some sulfuric acid, boiled off the water and distilled over the dimethyl dioxane.
However my yield was terrible, most of it converted to tar.
My original propylene glycol must have had impurities in it that encouraged tar formation.
So I proceeded to distill and purify all of my propylene glycol first.
It has a high boiling point of 183 celsius and doesn't form azeotropes with water, so purification was rather straightforward if slow.
At the end of the distillation i had a lot of residue leftover, this would explain the excessive tar formation.
So now with my purified propylene glycol i proceeded again to perform an acid catalyzed condensation reaction and produced dimethyl dioxane.
This time it worked a lot better and produced a much higher yield than before.
Okay, so far so good.
Following the old procedure to make regular dioxane i added some acid to hydrolyze side products and proceeded to distill it again.
Unfortunately this backfired spectacularly.
It turns out that dimethyl dioxane is highly susceptible to acid catalyze hydrolysis,
much more so than regular dioxane on which this procedure is based.
I ended up destroying most of my dimethyl dioxane and remaking propylene glycol as well as tar.
Learning from that blunder i repeated my synthesis and spent another couple of days making dimethyl dioxane again.
This time, to purify it i mixed it with potassium hydroxide and attempted base catalyzed hydrolysis of impurities.
Turns dimethyl dioxane is much more resistant to bases.
Now I know there are some impurities that are also resistant to bases
but i figured that if they could resist reacting with potassium hydroxide
then they would also likely resist reacting with the sodium hydroxide and magnesium metal reaction mixture.
So i proceeded to distill my reaction mixture.
Unfortunately the lab gods decided to make an example of me again and ruined the fractional distillation
by causing it to foam so much that it actually reached up the 150cm fractional distillation column and spill over.
Needless to say i was very disappointed.
Fractional distillations take hours to do and when there is a major upset like this you have to start all over again.
Eventually after a few more false starts, i distilled again with much smaller quantities and using larger apparatus to contain the foaming.
I was able to obtain dimethyl dioxane.
Unfortunately my bad luck didn't stop there.
It turns out the boiling point for dimethyl dioxane is around 117 celsius.
That's not much better than regular dioxane.
It probably wouldn't give any significant improvement.
But to be absolutely certain it wouldn't work i ran the reaction anyway and again, nothing happened.
This was a dead end.
All of that work and failure for nothing.
Do you guys still want me edit a video on how to make dimethyl dioxane even though it's useless? I have all the footage.
Let me know in the comments.
Anyway, that was my progress for making sodium this month.
Needing a diversion so i didn't go on a homicidal rampage from the frustration,
i decided to put that project on the back burner and revisit my pyrimethamine synthesis.
To round out the original video i wanted to product it using lab chemicals.
Rather than using the original domestic chemical route that's more complicated than NFL play night analysis.
If we could use lab chemicals then this much simpler two step route should be accessible.
So i've already begun work on the first step, performing the grignard reaction between ethyl magnesium bromide and p-chlorophenyl acetonitrile.
It seems to be working, but i won't know for certain until i run the nuclear magnetic resonance spectroscopy analysis.
I'm still processing this reaction.
So that's what i've been up to for the month of June.
sorry there are no actual videos.
I think i'm going to rename these progress report videos to Lab Note videos.
I think that better describes what they are as i'd also like to incorporate separate experiments, abandoned experiments and tangents.
Basically a video version of what you find in a lab notebook.
Ah well, let me know what you think.
And apologies again for june being a relatively dead month.