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>> No.7402943 [View]
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7402943

>>7402841
I've never actually done this reaction. I'm pretty sure you can just blast it with a general blacklight though.

>>7402845
Yup. There are other options too though, LDA is actually really nasty and you could probably just use NaOH.

After the bromination you're probably going to get a little bit of di-brominated product too. You could just ignore this for the next reaction (and just add heavy excess of ethyl acetate).

From this step, you would have the products in pic related.

I would personally just recrystallize at this step, assuming the di- product is minor. If it's a significant amount then the obvious solution is a column but you might be able to get around that by playing with trituration and shit.

In my opinion you should have pure mono- product before you de-esterify. After the reaction, I would extract with aqueous saturated bicarb solution to neutralize whatever acid I chose to use (let's say sulfuric), as well as remove some of the ethanol by-product. You could keep extracting with water to help get rid of the ethanol, though honestly you could probably just leave it on the rotovap or vacuum pump for a while and it will fuck off.

All of this is under the assumption that phenibut is solid.

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