In this video we'll be performing a famous condensation reaction between an

aromatic aldehyde, the nitroalkene called the Henry reaction.

We'll be using vanillin and nitrolethane and condensing these together to synthesize

the 2-nitrolypropan compound.

Start by weighing out 5 grams of dry vanillin crystals.

Note that there are many different ways to perform this reaction and if you want to use

a different aldehyde or nitroalkane.

You'll need to do some research and hunt out the best way.

Next, weigh out 2 grams of anhydrous ammonium acetate crystals.

These must be anhydrous.

Do not attempt to evaporate the mixture of aqueous ammonia and acetic acid.

Unfortunately it will not work.

Ammonium acetate is hygroscopic so heat this wrapped up to stop it absorbing moisture.

Measure out 3.5 grams of nitrolethane.

Check out our other video linked here for details about how this can be synthesized.

First add the vanillin to the nitrolethane in a 100 ml flask.

You'll immediately see a slight yellow color being produced.

Next, add the anhydrous ammonium acetate.

This will help the anhydrous ammonium acetate.

You can see the yellow color becoming more intense.

This is our reaction starting.

Now measure out 10 mils of glacial acetic acid.

This will act as a solvent for the reaction.

Add this to the flask.

The smoke produced is just some polylimonia from our catalyst reacting with the acetic

acid.

Give the mixture a good stir.

Most of the solids should dissolve.

Cover the top of the flask with plastic wrap.

We could now simply reflux the mixture but since we're doing this on a small scale we'll

do something a bit more cool.

Place the flask into a microwave oven.

We're using a regular kitchen microwave here.

Now microwave it in short bursts.

At 100 watts low power.

You want to get the liquid hot, but not boiling.

After the first 30 second burst the solids have dissolved and the liquid is turning an

orange color.

We allowed the flask to cool slightly and then placed back into the microwave.

There's a little bit of reflux in the flask, but no actual boiling occurring.

Perfect.

This is what we want.

We gave the flask about 7 minutes of total microwave exposure time over about a 30 minute

period.

Here's our flask at the end of the reaction.

Too much red color means impurities such as timers forming.

Let this rest for a few minutes, but don't allow to cool.

Prepare 35 grams of ice in a beaker.

The ice is now completely cold.

Now add the reaction mixture to this.

Kelly can silent but here I am át Strøde the mixture well, and watch out the

reaction flask with 10 mls of cold water.

Adding this to the beaker, the oil present in the mixture should pretty rapidly crystallize

into a yellow precipitate.

You can see lots of crystals where we scratched the glass.

I'll move this over into a蒶 duckón before haying a metal nail into it.

We allowed the crystalline precipitate to settle and then set up for filtration.

We washed the beaker and the precipitate with 20 mils of cold water.

And got the crude product as dry as we could using the filter pump.

Here's our crude product 3.2 grams of a yellow crystalline solid with only a very faint aroma of vanillin.

This is a slightly disappointing 47% yield, so either we needed to use a bit more time in the microwave,

or perhaps this is best done using a slow rewound.

We re-crystallized this using a mixture of 40% water in 60% methanol by volume.

It took about 25 mils of hot solvent to get all the crude product to dissolve.

On cooling, as the product crystallized out of the solution, some amazing patterns were seen dancing in the liquid.

The mixture was then chilled down for 30 minutes to allow everything to crystallize out.

The crystals were really beautiful as you can see.

These were filtered off and dried with 20 mils of cold water, then allowed to dry thoroughly on the pump.

And here's our purified product.

This is a physical area, you see there's only one help spot, two simple bombs going through there for surface damage process.

2.8 grams of the vanilla nitrile faire obedience.

condensation and elimination product.

This compound is relatively unstable and you'll need to keep it in the freezer if you want

to store it for more than a day or two.

It decomposes readily in contact with warm water to produce red colored decomposition products.

For more information visit www.fema.gov