4mmc synthes in ethyl acetate
- Thread starter The Villain
- Start date
video says:
- no heating
- 20 minutes reaction time
- color changes very visible
my experience is :
- keep at 40
- 30 minutes reaction time
- color changes are subtle, but at some point it will turn brown (when dark yellow, just wait more).
- no heating
- 20 minutes reaction time
- color changes very visible
my experience is :
- keep at 40
- 30 minutes reaction time
- color changes are subtle, but at some point it will turn brown (when dark yellow, just wait more).
is this timeframe without using triethylamine?
Just 2b4m,methylamine and ethyl acetate?
as far as i understand, ethyl acetate makes the reaction much faster than DCM, correct me if am wrong.
Just 2b4m,methylamine and ethyl acetate?
as far as i understand, ethyl acetate makes the reaction much faster than DCM, correct me if am wrong.
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- By TheVacuumGuy
Yes. Without triethylamine.
But despite its speed, this is not a route I use regularly.
But despite its speed, this is not a route I use regularly.
you don't prefer it due to lower yields?
also what is the average yield someone should expect from using EA?
also is the acidification procedure the same as with using DCM when using EA?
also what is the average yield someone should expect from using EA?
also is the acidification procedure the same as with using DCM when using EA?
- By TheVacuumGuy
I dont care about yield percentage game since it's all margins talk. I'll explain below.
To your question: when done correctly, ~55% is possible.
Acidification process is more or less the same.
Check out the Video (and thread), and New thread
More than yields, I care about failures. And in ethylacetate ( even more than in DCM ) , risk of screwing it up are higher. When using ethylacetate as your reaction solvent, acidification can result in a dark mess, and/or no precipitate (+ a full trashcan). In terms of yield that is 0.
Any other method which gives only 30% yield, but is more robust, is a clear winner imho.
However, ethylacetate is life saver when using DCM as the reaction solvent, to replace acetone for acidification, which reduces the chance of bright colored paint in your product to nearly zero.
But doing so comes with a price, which is (when not having some pro drying equipment) harder to dry your product in a timely and correct matter, causing tinted crusts which needs removal before crystallization (or just crush, but better to cut those away (inside is nice white, but moist, powder).
To your question: when done correctly, ~55% is possible.
Acidification process is more or less the same.
Check out the Video (and thread), and New thread
More than yields, I care about failures. And in ethylacetate ( even more than in DCM ) , risk of screwing it up are higher. When using ethylacetate as your reaction solvent, acidification can result in a dark mess, and/or no precipitate (+ a full trashcan). In terms of yield that is 0.
Any other method which gives only 30% yield, but is more robust, is a clear winner imho.
However, ethylacetate is life saver when using DCM as the reaction solvent, to replace acetone for acidification, which reduces the chance of bright colored paint in your product to nearly zero.
But doing so comes with a price, which is (when not having some pro drying equipment) harder to dry your product in a timely and correct matter, causing tinted crusts which needs removal before crystallization (or just crush, but better to cut those away (inside is nice white, but moist, powder).
- By Dr. MMX
I do have a feeling that EA is easiest solvent, literally always clean job. I dont know what happened that you say its easy to do mistake. I think just patient 1 drop a sec on acidification gives always good result. If somebody is hurry and will change its dripping rate then its real risk to fail - its true
I did successful acidification on DCM using acetone, color was almost white - as well 1 drip of acid per sec, but when i tried ethyl acetate another time it was while so I admit using acetone is harder with DCM, but in general acetone has its advantages.
Both cases i didnt get really sucessful yield, as i remember about 50% (dcm) but I dont really remember what I did exactly becasue it was while ago and I was testing some "new things"
I did successful acidification on DCM using acetone, color was almost white - as well 1 drip of acid per sec, but when i tried ethyl acetate another time it was while so I admit using acetone is harder with DCM, but in general acetone has its advantages.
Both cases i didnt get really sucessful yield, as i remember about 50% (dcm) but I dont really remember what I did exactly becasue it was while ago and I was testing some "new things"
- By TheVacuumGuy
Sidenote: I have no degree in chemistry.
What I described above is just my experience and may, or may not be, scientifically correct.
What I described above is just my experience and may, or may not be, scientifically correct.