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Using the Grignard Reaction to Make Tertiary alcohols
In this video we make tertiary alcohols using the (in)famous Grignard reaction.
Briefly, an alkyl halide is reacted with magnesium metal to form an organometallic alkyl magnesium halide. This is the grignard reagent. This reagent is then reacted with a carbonyl containing compound suck as a ketone, an ester or an organic carbonate to form a tertiary alcohol. The mixture is then reacted with water and titrated with acid to dissolve the magnesium hydroxides formed. Finally, the alcohol is purified by a series of liquid extractions and distillations.
Related videos:
Purifying and drying diethyl ether for use in grignard reactions: https://www.youtube.com/watch?v=EEXqjJd0Bak
Making alkyl halides: https://www.youtube.com/watch?v=Ydn1D4FSqkc
...
https://www.youtube.com/watch?v=EFQWD7-DCPI
Briefly, an alkyl halide is reacted with magnesium metal to form an organometallic alkyl magnesium halide. This is the grignard reagent. This reagent is then reacted with a carbonyl containing compound suck as a ketone, an ester or an organic carbonate to form a tertiary alcohol. The mixture is then reacted with water and titrated with acid to dissolve the magnesium hydroxides formed. Finally, the alcohol is purified by a series of liquid extractions and distillations.
Related videos:
Purifying and drying diethyl ether for use in grignard reactions: https://www.youtube.com/watch?v=EEXqjJd0Bak
Making alkyl halides: https://www.youtube.com/watch?v=Ydn1D4FSqkc
...
https://www.youtube.com/watch?v=EFQWD7-DCPI
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By popular request, how to make Copper (II) Chloride.
The first and simplest method is to get hydrochloric acid of around ~20% concentration and add copper. Then bubble air through it using an aquarium pump. The oxygen in the air oxidizes the copper and reacts with the acid to produce copper chloride. Pretty much any concentration of acid can be used, but we recommend around 20% as there are considerably less fumes. A major drawback of this method is that it's VERY slow and can take days to produce useful quantities of copper chloride.
The second far faster method is to react hydrochloric acid and copper with an equal volume of hydrogen peroxide. The recommended concentration of acid is greater than 20% and the peroxide is equal or greater than 3%. In our video we used 200 mL 31% hydrochloric acid, 30g of copper and 200 mL of 6% hydrogen peroxide. This reaction only takes a few hours to finish.
For many applications like PCB etching or gold recovery from circuit boards, sulfate contamination is not a problem so the third method uses readily available copper sulfate. Just take the copper sulfate and add as much hydrochloric acid as necessary to dissolve it. This directly produces copper chloride that can be used for the previously mentioned application. It will be contaminated with sulfate ions but these have no effect.
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The vacuum is provided by powerful aspirator vacuum pump and the concept is explored in our own video on an amateur version of the same system: https://www.youtube.com/watch?v=tYLlkTDstmo
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First, spray the car starter fluid into a flask. Setup a fractional distillation apparatus around the flask but cool the condenser with ice water. Diethyl ether boils at 34.6 degrees Celsius so a room temperature condenser wouldn't be as efficient as an ice temperature condenser. Now start with very light heating and gradually ramp up until diethyl ether starts to distill at 34 celsius or so. Go slowly at first as diethyl ether boils very easily. You'll need to gradually increase the temperature to keep the flow constant. Eventually there will be a spike in distillate temperature as the ether finishes distilling so stop the heating if it passes 70 celsius. The collected product diethyl ether while the residue should be other aliphatic solvents. Most starter fluids contain heptane in addition to ether.
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Related Videos:
Making tertiary alcohols by the Grignard Reaction: https://www.youtube.com/watch?v=EFQWD7-DCPI
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