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unlikely that 20gr of MgSO4 caused such a disaster. is your roluene mix still basic or neutral? Ethylacetate works perfectly for gassing.

They rely on a very low solubility of ammonium chloride in butyl alcohol. The reaction after step 4 will contain a huge amount of ammonium chloride. You can cool it down after step 4, precipitate unreacted ammonium chloride, filter it out, then reduce liquid volume twice by gentle boiling, then...

if your powder is not water soluble then you have either acid or ester. Both can be converted to the salt by treating it with NaOH just as described in the very first message of this topic. Step 1.

I have no idea how they guys on this video got the yeld they got. My experiments with HCl were low yelding. You need reflux temperature, huge excess of an acid (1:3 by weight) , good stirring and long reaction time. Some people say they have success with HCl. I only had success with phosphoric...

1 mol of alkali to 1 mol of adduct.

Dissolve 0.5 mol of sodium metabisulphite in small amount of water. Near saturated solution. Dissolve your aldehyde in x2-x3 volumes of ethyl acetate. Put it all together in a flask with mechanical stirring. Wait until you get thick white goo. Mix it few hours for complete conversion. Filter...

salt is water soluble. acid and glycidate are not. salt has pretty high melting point, acid and glycidates are below 100 degrees

https://bbgate.com/threads/phenylacetone-p2p-synthesis-from-benzaldehyde-with-butanone.187/page-7#post-35597

See post #121 above on this page

You can use aqueous HCl. Just use 1 liter of benzaldehyde to 2 liters of MEK and calculated amount of 35..37% hydrochloric acid. You need 20g of PURE HCl per each 100g of benzaldehyde. So 1L of benzaldehyde will require 200g of PURE HCl. Now calculate how much aqueous acid do you need. With...

Yes thats true. Thats why I said "cafrefully evaporate". And of course it is must not be done in a closed room. Without professional equipment it is better done with all windows open and a fan blowing vapours straight to the window. Or just stick to nitrate salt. However I usually evaporated it...

HCl will not replace nitric in Hg nitrate as nitric is stronger than HCl. If I understood you right :). You either have to react metallic mercury with nitric acid to get a nitrate and use it as is or get a nitrate, then basify it with NaOH to get a mercury oxide (precipitates) then react the...

So at what step an excess of methylamine is removed? How you can be sure that methylamine hcl is not in final product? Just curious

no sulphates can not be smoked. it will decompose before evaporation

So far: 1. HCl only 37% + water solution of 5449: no decarboxylation visible up to reflux, zero yeld, just some phenylacetone smell 2. H2SO4 30% + water solution of 5449 : very low yeld 3. HCl 37% + oxalic acid + + water solution of 5449 : no decarboxylation reaction up to 85 degrees, zero...

40ml crude P2P yelded 2..3ml of P2P. . 100g of powder yelded 3ml. Ok enough of HCl experiments, lets try phosphoric and then dump all that 5449 I got to the drain. Never thought it can be so annoying.

Aha :). Looks like my failures were all related to incomplete decarboxylation reaction. Which may be caused by insufficient stirring and/or reaction time. This time I got 40ml of crude p2p from 100g of powder (just top layer collected). Then I extracted water layer with DCM twice and added...

Does anyone have a pic of how decarb. bubbling should look like?

Last experiment with sulphuric acid, I stop playing with it, too upsetting : 1. 20g of powder was dissolved in 30ml of water with stirring 2. 25g of sulphuric acid 98% was dissolved in 40ml of water and cooled to room temperature While stirring at 1500rpm acid was slowly added to glycidic acid...

oh, I made a mistake. I mean 80ml of water + 20g of sulphuric. This was added to powder which was dissolved in 30ml of warm water. Stirred in 250ml flask on a magnetic stirrer, 1500rpm, temp of the oil bath was 70 degrees.